WO2014156694A1 - Particulate-measuring method, particulate-measuring system, and system for manufacturing ultrapure water - Google Patents

Particulate-measuring method, particulate-measuring system, and system for manufacturing ultrapure water Download PDF

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Publication number
WO2014156694A1
WO2014156694A1 PCT/JP2014/056747 JP2014056747W WO2014156694A1 WO 2014156694 A1 WO2014156694 A1 WO 2014156694A1 JP 2014056747 W JP2014056747 W JP 2014056747W WO 2014156694 A1 WO2014156694 A1 WO 2014156694A1
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Prior art keywords
unit
measurement
abnormality
filter
fine particle
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PCT/JP2014/056747
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French (fr)
Japanese (ja)
Inventor
田中　洋一
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栗田工業株式会社
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Application filed by 栗田工業株式会社 filed Critical 栗田工業株式会社
Priority to CN201480017748.0A priority Critical patent/CN105051519A/en
Priority to US14/778,872 priority patent/US20160047730A1/en
Priority to KR1020157030224A priority patent/KR20150136606A/en
Publication of WO2014156694A1 publication Critical patent/WO2014156694A1/en

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/06—Investigating concentration of particle suspensions
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/008—Control or steering systems not provided for elsewhere in subclass C02F
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/06—Investigating concentration of particle suspensions
    • G01N15/0606—Investigating concentration of particle suspensions by collecting particles on a support
    • G01N15/0618—Investigating concentration of particle suspensions by collecting particles on a support of the filter type
    • G01N15/0625—Optical scan of the deposits
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/36—Organic compounds containing halogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/02—Non-contaminated water, e.g. for industrial water supply
    • C02F2103/04—Non-contaminated water, e.g. for industrial water supply for obtaining ultra-pure water
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00—Controlling or monitoring parameters in water treatment
    • C02F2209/005—Processes using a programmable logic controller [PLC]
    • C02F2209/006—Processes using a programmable logic controller [PLC] comprising a software program or a logic diagram
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00—Controlling or monitoring parameters in water treatment
    • C02F2209/10—Solids, e.g. total solids [TS], total suspended solids [TSS] or volatile solids [VS]
    • C02F2209/105—Particle number, particle size or particle characterisation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/10—Devices for withdrawing samples in the liquid or fluent state
    • G01N2001/1006—Dispersed solids
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N2015/0042—Investigating dispersion of solids
    • G01N2015/0053—Investigating dispersion of solids in liquids, e.g. trouble
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/00584—Control arrangements for automatic analysers
    • G01N35/00594—Quality control, including calibration or testing of components of the analyser
    • G01N35/00712—Automatic status testing, e.g. at start-up or periodic

Definitions

  • the present invention relates to a fine particle measurement method and a fine particle measurement system used for measuring fine particles in sample water.
  • pure water including ultrapure water
  • various industrial fields such as the semiconductor manufacturing field and the pharmaceutical manufacturing field.
  • the demand for the quality of pure water used in the industrial field has been increasing in recent years, and inspection and management are performed to confirm that the required water quality is maintained in primary pure water production equipment and ultrapure water production facilities. It has been broken.
  • one of the water quality management items is the number of fine particles contained in 1 ml of pure water.
  • Patent Document 1 discloses an ultrapure water production apparatus including a fine particle meter that measures the number of fine particles, a TOC meter that measures a TOC (total organic carbon content) value, a specific resistance meter that measures a specific resistance value, and the like. It is disclosed.
  • Patent Document 2 describes a method and apparatus for measuring the number of fine particles in ultrapure water by filtering ultrapure water with a filter and counting the number of fine particles adhering to the filter with a microscope. .
  • This method of measuring the number of fine particles is called a direct spectroscopic method, and is usually used for performing a detailed analysis of fine particles during periodic inspections or abnormal times.
  • the on-line particle counter has the advantage that it can easily measure the fine particles in pure water on-time, and from this advantage, daily particle management is performed to monitor the number of fine particles in pure water.
  • the on-line type fine particle counter the smaller the particle size of the fine particles, the more difficult the measurement in real time becomes, and the more difficult the measurement is with respect to the increasing required water quality.
  • the direct spectroscopic method detailed analysis is possible and measurement that satisfies the required water quality is possible, but real-time measurement is not possible and analysis takes time. For this reason, as described above, it is common sense that the direct spectroscopic method is used only during periodic inspections or when abnormalities such as measurement of a predetermined number or more of particles are confirmed by the particle counter. It has been.
  • the present invention provides a fine particle measurement method and a fine particle measurement system that can capture fine particles in sample water in a timely manner even in a situation where an abnormality is recognized in the measurement result by the measurement unit that measures the fine particles in sample water.
  • the main purpose is to do.
  • the present invention operates both a measurement unit that measures fine particles in sample water and a filtration unit that filters the sample water and captures the fine particles for direct spectroscopic analysis.
  • a fine particle measurement method in which even when an abnormality is found in a measurement result, the step of continuously filtering the sample water is performed.
  • the measurement unit and the filtration unit for analysis by the direct spectroscopic method are operated together, and even if an abnormality is recognized in the measurement result of the measurement unit, the sample water is continued. Since filtration is performed, it becomes possible to capture fine particles in a timely manner even when an abnormality occurs.
  • the step of continuously filtering the sample water can be performed by continuously operating the filtration unit. it can.
  • the filtration unit includes a first filtration unit and a second filtration unit that are installed so that the supply of the sample water can be switched, and the measurement unit and the first filtration unit. In the state where both are in operation, when an abnormality is recognized in the measurement result by the measurement unit, the first filtration unit is stopped and the second filtration unit is operated, thereby continuously A step of filtering the sample water can be performed.
  • the filtration unit that is continuously filtered after an abnormality is recognized in the measurement result by the measurement unit can be stopped after the abnormality is resolved. Then, it is possible to analyze the fine particles captured by the filtration unit that is continuously filtered after an abnormality is recognized in the measurement result by the measurement unit.
  • the analysis of the fine particles can be performed by a so-called direct spectroscopic method in which measurement is performed using an optical microscope or a scanning electron microscope.
  • the present invention also includes a measuring unit that measures fine particles in sample water, a filtering unit that filters the sample water and captures the fine particles for analysis by direct spectroscopic method, and both the measuring unit and the filtering unit.
  • a fine particle measurement system comprising: a control unit that performs control so that the sample water is continuously filtered when an abnormality is found in the measurement result of the measurement unit in an operating state. .
  • the control unit can continuously operate the filtering unit even when an abnormality is recognized in the measurement result by the measuring unit.
  • the filtration unit includes a first filtration unit and a second filtration unit that are installed so that the supply of the sample water can be switched, and the control unit operates with both the measurement unit and the first filtration unit.
  • the first filtration unit When the abnormality is recognized in the measurement result by the measurement unit, the first filtration unit can be stopped and the second filtration unit can be operated.
  • the said control part can stop the filtration part currently filtered after abnormality is recognized by the measurement part by the said measurement part, after the said abnormality is eliminated.
  • the control unit can determine that the abnormality is detected when the measurement unit continuously measures the fine particles for a predetermined number or more and for a predetermined time.
  • the present invention provides an ultrapure water production system comprising the fine particle measurement system according to the present invention in a pure water production process.
  • a fine particle measurement method and a fine particle measurement system capable of capturing fine particles in a sample water in a timely manner even in a situation where an abnormality is found in the measurement result of the measurement unit that measures the fine particles in the sample water. Is done.
  • 1 is a system diagram showing an example of the configuration of a particle measuring system to which a particle measuring method according to a first embodiment of the present invention is applied. It is a flowchart figure showing the particulate measuring method of a 1st embodiment of the present invention. It is a systematic diagram which shows the example of 1 structure of the fine particle measurement system to which the fine particle measurement method of 2nd Embodiment of this invention is applied. It is a flowchart figure showing the particulate measuring method of a 2nd embodiment of the present invention. It is a systematic diagram which shows the structural example of the ultrapure water manufacturing equipment to which the fine particle measurement system of this invention is applied.
  • the fine particle measurement method includes a measurement unit that measures fine particles in sample water, and a filtration unit that filters the sample water and captures the fine particles for analysis by direct microscopic analysis. The process of continuously filtering the sample water is performed even when an abnormality is found in the measurement result by the section.
  • the step of continuously filtering the sample water is performed even when the measurement unit and the filtration unit are both in an operating state and an abnormality is recognized in the measurement result of the measurement unit. Is called. Therefore, it is possible to capture fine particles in the sample water in a timely manner even when the measurement result by the measurement unit is abnormal.
  • the fine particles can be captured in a timely manner, the number of fine particles that are not captured (the number of losses) can be suppressed, and the amount of captured fine particles can be increased.
  • the captured fine particles can be analyzed in detail by direct spectroscopic methods. Therefore, in the fine particle measurement method according to the present disclosure, it is possible to quickly identify the cause of the abnormality in the measurement result by the measurement unit, and it is possible to improve the quality of fine particle management in pure water.
  • the fine particle measurement method of the present disclosure includes a process (procedure) in the method, for example, a CPU of an apparatus (for example, a personal computer or the like) for managing the size (particle diameter) and the number of fine particles to be measured. It is also possible to store it as a program in a hardware resource including a control unit and a storage medium (USB memory, HDD, CD, etc.) and realize the program by the control unit.
  • a process in the method, for example, a CPU of an apparatus (for example, a personal computer or the like) for managing the size (particle diameter) and the number of fine particles to be measured.
  • a hardware resource including a control unit and a storage medium (USB memory, HDD, CD, etc.) and realize the program by the control unit.
  • the fine particle measurement method of the present disclosure can be executed by being applied to a fine particle measurement system including a control unit.
  • This fine particle measurement system is operated by a measurement unit in a state where a measurement unit that measures fine particles in sample water and a filtration unit that filters sample water and captures the fine particles for direct spectroscopic analysis are in operation. And a control unit that controls the sample water to be continuously filtered when an abnormality is found in the measurement result.
  • the fine particle measurement method and the fine particle measurement system of the present disclosure can be applied to a primary pure water production system, and more preferably, ultrapure water production that further purifies pure water produced by the primary pure water production system. It can be applied to a system (also referred to as a secondary pure water production system and a subsystem).
  • the primary pure water production system is an apparatus for finishing to pure water, and examples thereof include an ion exchange resin, a reverse osmosis membrane, or a combination thereof.
  • the secondary pure water production system is configured by combining, for example, a heat exchanger, an ultraviolet oxidation device, an ion exchange device, and an ultrafiltration device.
  • sample water that is the target of the fine particle measurement method and the fine particle measurement system of the present disclosure is not particularly limited.
  • the pure water in the production process of the primary pure water production system and the ultrapure of the secondary pure water production system examples include ultrapure water in the water production process.
  • the “sample water” includes water that is a target for removing impurities such as ionic components, organic substances, and fine particles.
  • both the fine particle measuring instrument as the measuring unit and the filter as the filtering unit are operated together, and even when an abnormality is recognized in the measurement result of the fine particle measuring instrument, By continuously operating the filter, the filtration is continuously performed.
  • FIG. 1 is a system diagram showing a configuration example (a fine particle measurement system according to the first embodiment) of a fine particle measurement system to which the fine particle measurement method of the present embodiment is applied.
  • the fine particle measurement system 11 according to the present embodiment includes a fine particle measurement device 12, a filter 13, and a control unit 14.
  • the particle measuring instrument 12 and the filter 13 are branched and connected from a pipe 16 through which sample water (pure water in the present embodiment) W stored in the storage tank 15 flows.
  • the fine particle measuring instrument 12 receives pure water W from the pipe 16 and measures at least the number of fine particles in the pure water.
  • the fine particle measuring instrument 12 of the present embodiment can continuously measure the number and size (particle size) of fine particles in pure water.
  • the fine particle measuring device 12 measures fine particles in accordance with “Measurement method using automatic fine particle measuring device” in JIS K0554 (fine particle measuring method in ultrapure water).
  • the fine particle measuring device 12 outputs the number of fine particles in water per unit volume (unit: piece / ml) to the monitor as a measurement value, and always measures and monitors the number of fine particles in pure water on time (real time). . Then, the particle measuring instrument 12 confirms whether or not an abnormality is recognized in the number of particles as a measurement result.
  • the “abnormality” in the measurement result by the particle measuring instrument 12 is set from the particle diameter and number of the measured particles, the confirmed time, and the like according to the required water quality. For example, a case where a predetermined number of fine particles or more are confirmed by a fine particle measuring instrument 12 for a predetermined time or more can be set as “abnormal”.
  • the “predetermined number” of fine particles measured by the fine particle measuring instrument 12 can be set, for example, from a range of 100 to 10,000 / L (preferably 500 to 5000 / L).
  • the “predetermined time” can be set, for example, in the range of 30 seconds to 30 minutes (preferably 1 minute to 10 minutes). In these ranges, one specific example that can be suitably set in the ultrapure water production system is as follows. For example, when the fine particle measuring device 12 continuously confirms, for example, 1000 particles / L or more fine particles for 5 minutes or more, “ “Abnormal” can be set.
  • the filter 13 filters the pure water W introduced from the pipe 16 and captures fine particles for analysis by a direct spectroscopic method, and includes a filtration membrane for capturing the fine particles.
  • the filter 13 is for capturing fine particles with a filtration membrane and analyzing them directly by a microscopic method even for fine particles having such a small particle diameter that it is difficult to measure with the fine particle measuring instrument 12.
  • the direct microscopic method for example, the size (particle diameter), number, composition, and the like of fine particles can be analyzed.
  • the filter 13 is not particularly limited as long as the fine particles in the pure water W can be captured by the filtration membrane.
  • a centrifugal filter and a separation membrane unit using a water pressure can be used.
  • the separation membrane unit using the water passage pressure is a unit having a separation membrane (filtration membrane) and having a structure in which the power of filtration is based on the water passage pressure. Since the power of filtration depends on the water flow pressure, it takes time to pass the water in order to earn the necessary amount of filtered water, but it is preferable because it can be easily installed.
  • the centrifugal filter uses centrifugal force for filtration, the centrifugal filter is more preferable because a necessary amount of filtered water can be obtained in a shorter time than a separation membrane unit using a water flow pressure.
  • the centrifugal filter 13 is used as the filter 13.
  • the filtration time by the filter 13 used in the fine particle measurement method and the fine particle measurement system 11 of the present disclosure is not particularly limited, and is appropriately set according to the required water quality. For example, when measuring 1 minute / ml of particles having a particle size of 0.05 ⁇ m or more as the required water quality, it is desirable that the centrifugal filter has a pressure of 2 MPa and 20 days or more, and the filtration by water pressure sets the pressure to 0.4 MPa. In some cases, 100 days or more is desirable.
  • the said filtration time is fluctuate
  • the filtration membrane used for the filter 13 can use the commercial item used in the normal pure water manufacture field
  • the filtration membrane is not particularly limited as long as it has a structure capable of capturing fine particles to be measured on the surface and allowing sample water to pass therethrough.
  • the types of filtration membranes by pore size include microfiltration membranes (MF membranes), ultrafiltration membranes (UF membranes), and reverse osmosis membranes (RO membranes).
  • MF membranes microfiltration membranes
  • UF membranes ultrafiltration membranes
  • RO membranes reverse osmosis membranes
  • Examples of the structure of the filtration membrane include a hollow fiber membrane, a spiral membrane, and a tubular membrane.
  • Examples of the material of the filtration membrane include cellulose acetate, aromatic polyamide, polyvinyl alcohol, polyvinylidene fluoride, polyethylene, polyacrylonitrile, polypropylene, polycarbonate, polytetrafluoroethylene, and ceramic.
  • the control unit 14 has a function of controlling at least the filter 13.
  • the control unit 14 continues to operate the filter 13 even when an abnormality is found in the measurement result by the particle measuring instrument 12 in a state where both the particle measuring instrument 12 and the filter 13 are operating. It is a part which controls so that filtration of pure water may be performed continuously.
  • the control unit 14 may be provided in the filter 13 or may be provided separately from the filter 13.
  • control unit 14 may have a function of controlling the particle measuring instrument 12 in addition to the filter 13.
  • the particle measuring instrument 12 and the control unit 14 cooperate to output a measurement result by the particle measuring instrument 12 to the control unit 14, and the control unit 14 determines whether or not the measurement result is abnormal. Also good.
  • the control unit 14 determines whether or not the measurement result is abnormal. Also good.
  • the normal value and the abnormal value of the measurement result are stored in a storage medium cooperating with the control unit 14, and the control unit 14 stores the measurement value in the storage medium. The determination can be made based on the normal value and abnormal value data of the result.
  • the control unit 14 has a predetermined number or more of the particles. It is preferable to determine that there is an abnormality when measured continuously for more than a time. Thereby, only the reliable abnormality resulting from the number and size of the fine particles by the fine particle measuring instrument 12 can be determined.
  • the “predetermined number” and the “predetermined time” can be set within the range described in the “abnormality” in the measurement result by the fine particle measuring instrument 12 described above. The same applies to “predetermined number” and “predetermined time” described later.
  • FIG. 2 is a flowchart showing the fine particle measurement method of the present embodiment.
  • this flowchart figure also represents operation
  • FIG. 2 as a premise that the fine particle measurement method of the present embodiment is started, a state where pure water W is introduced into the fine particle measuring instrument 12 and the filter 13 is started.
  • both the particle measuring device 12 and the filter 13 are operated (step S11).
  • the particle measuring instrument 12 and the filter 13 do not necessarily have to be operated at the same time, as long as both the particle measuring instrument 12 and the filter 13 are in operation.
  • the operating state of the particle measuring device means a state in which sample water is introduced into the particle measuring device and the particles contained in the sample water are measured by the particle measuring device.
  • the operating state of the filter means a state in which pure water is introduced into the filter and sample water is filtered. At this time, when fine particles are contained in the sample water, the fine particles are captured.
  • rotation speed, pressure, and continuous operation time (one cycle continuous operation time, days) of the filter 13 depend on the target sample water, the place where the particulate measurement method according to the present disclosure is applied, and the like. Are appropriately selected.
  • step S12 presence / absence of abnormality in the measurement result by the particle measuring instrument 12 is confirmed (step S12).
  • the presence or absence of this abnormality may be determined by the control unit.
  • the particle measuring instrument 12 and the control unit 14 cooperate to output a measurement result from the particle measuring instrument 12 to the control unit 14, and the control unit 14 determines whether or not the measurement result is abnormal. Can do.
  • the control unit 14 determines whether or not the measurement result is abnormal. Can do.
  • the control unit 14 for the determination of the presence / absence of abnormality by the control unit 14, for example, the normal value and the abnormal value of the measurement result are stored in a storage medium cooperating with the control unit 14 using a threshold value or a numerical range, and the control unit 14 stores the normal value. The determination can be made based on the normal value and abnormal value data of the measurement result stored in the medium.
  • the control unit 14 has a predetermined number or more of the particles. It is preferable to determine that there is an abnormality when measured continuously for more than a time. Thereby, only the reliable abnormality resulting from the number and size of the fine particles by the fine particle measuring instrument 12 can be determined.
  • step S12 When abnormality is confirmed by step S12, it filters by the filter 13 continuously (step S13). Even when no abnormality is confirmed in step S12, the fine particle measuring instrument 12 and the filter 13 remain in an operating state, and these are always operated (step S11). It should be noted that keeping the filter 13 in operation at all times includes keeping the filter 13 in operation continuously at an arbitrary time (number of days). After completion of one cycle of continuous operation of the filter 13, it is preferable to replace the filter membrane of the filter 13 within several tens of minutes (for example, 30 minutes) and continuously operate again.
  • the filter 13 that is continuously operating after an abnormality is confirmed in the measurement result by the particle measuring instrument 12 is stopped after a predetermined time (step S15).
  • the time for stopping the filter 13 is preferably set to the time when the abnormality is resolved in order to surely capture the abnormal particles by the filter 13 (step S14). In this case, it is preferable to determine whether or not the abnormality has been resolved so that the abnormality is resolved and the stop condition of the filter 13 is set. This determination can also be performed by the control unit 14.
  • the time when the filter 13 is stopped can be set after a predetermined time has passed after the abnormality is confirmed or after a predetermined amount of filtration has passed through.
  • the predetermined time or the predetermined filtration amount is preferably set to a time or a filtration amount sufficient for eliminating the abnormality, depending on the required water quality and the target sample water.
  • step S16 sample water (pure water) for which the number of fine particles is to be measured is filtered through a filtration membrane that can capture the fine particles of the desired size, and the fine particles are captured and counted with a microscope for observation. In this method, the number of fine particles present in the sample is obtained.
  • the measurement by the direct spectroscopic method is performed in accordance with “Measurement method using an optical microscope” or “Measurement method using a scanning electron microscope” in JIS K0554 (Method for measuring fine particles in ultrapure water).
  • the composition of the fine particles can be analyzed while observing the fine particles with a scanning electron microscope using an apparatus in which an X-ray analyzer such as an energy dispersive X-ray analyzer (EDX) is attached to the scanning electron microscope. .
  • EDX energy dispersive X-ray analyzer
  • the particle measuring instrument 12 and the filter 13 for analysis by the direct spectroscopic method are operated together to measure the particle.
  • the filter 13 is continuously operated, so that the fine particles can be captured in a timely manner in the event of an abnormality. Therefore, the number of fine particles that are not captured can be reduced, and the amount of captured fine particles can be increased.
  • the captured fine particles are analyzed in detail by a direct spectroscopic method, and it becomes possible to quickly investigate the cause of the abnormality in the measurement result by the fine particle measuring instrument 12, thereby improving the quality of fine particle management in pure water. It becomes possible.
  • the pure water introduced into the fine particle measuring instrument (measuring unit) 12 and the filter (filtering unit) 13 may be drained, passed through the recovery line, or the raw water tank or It collects in a turbidity water tank and may be used as a part of raw water.
  • the fine particle measurement method and the fine particle measurement system according to the second embodiment are different from the first embodiment in that two filters are used as a filtration unit that captures fine particles for analysis by a direct spectroscopic method.
  • the first filtration unit (first filter) and the second filtration unit are installed so that the supply of sample water (pure water in this embodiment) can be switched to each other.
  • a filtration unit (second filter) is used.
  • the particle measuring method of the present embodiment is the first when the measurement result by the particle measuring instrument is found to be abnormal while the particle measuring instrument and the first filter are operating as the measuring unit.
  • the first filter is stopped and the second filter is operated.
  • pure water is continuously filtered by using the first filter and the second filter.
  • FIG. 3 is a system diagram showing a configuration example of the fine particle measurement system 21 to which the fine particle measurement method of the present embodiment is applied (the fine particle measurement system 21 according to the second embodiment).
  • the fine particle measurement system 21 of the present embodiment includes a fine particle measuring instrument 12, a first filter 23a, a second filter 23b, and a control unit 24.
  • the particle measuring instrument 12, the first filter 23a, and the second filter 23b are branched and connected from the pipe 16 through which the sample water (pure water) W stored in the storage tank 15 flows.
  • the particle measuring instrument 12 used in the present embodiment is the same as the particle measuring instrument 12 used in the first embodiment.
  • the first filter 23a and the second filter 23b used in the present embodiment are both described in the same manner as the filter 13 used in the first embodiment, but are controlled by the control unit 24. This is different from the first embodiment.
  • the centrifugal filters 23a and 23b are both used as the first filter 23a and the second filter 23b, but other filters such as a separation membrane unit may be used.
  • the control unit 24 has a function of controlling at least the first filter 23a and the second filter 23b. And the control part 24 stops the 1st filter 23a, when abnormality is recognized in the measurement result by the particle measuring device 12, in the state which the particle measuring device 12 and the 1st filter 23a are working together.
  • the second filter 23b is operated to control the pure water W to be continuously filtered.
  • the control unit 24 may be provided in the first filter 23a and / or the second filter 23b, and may be provided separately from the first filter 23a and the second filter 23b.
  • control unit 24 may have a function of controlling the particle measuring instrument 12.
  • the particle measuring instrument 12 and the control unit 24 cooperate to output a measurement result from the particle measuring instrument 12 to the control unit 24, and the control unit 24 determines whether or not the measurement result is abnormal. Can do.
  • the particle measuring instrument 12 and the control unit 24 cooperate to determine whether the measurement result by the particle measuring instrument 12 is abnormal or not accurately and quickly.
  • the control unit 24 In the determination of the presence or absence of abnormality by the control unit 24, for example, the normal value and the abnormal value of the measurement result are stored in a storage medium cooperating with the control unit 24, and the control unit 24 stores the measurement value in the storage medium. The determination can be made based on the normal value and abnormal value data of the result. Further, in consideration of the case where the abnormality of the measurement result by the particle measuring instrument 12 is resolved immediately or the case where the abnormality due to the defect of the particle measuring instrument 12 itself is confirmed, the control unit 24 has a predetermined number of particles more than a predetermined number. It is preferable to determine that there is an abnormality when measured continuously for more than a time. Thereby, only the reliable abnormality resulting from the number and size of the fine particles by the fine particle measuring instrument 12 can be determined.
  • the control unit 24 stops the second filter 23b that has been operated in order to continuously perform filtration, and the first filter 23a that has been stopped. Can be controlled to operate again.
  • the control unit 24 controls the first filter 23a and the second filter 23b in this way, and the measurement result by the fine particle measuring device 12 is normal, the first filter 23a performs filtration.
  • the measurement result by the fine particle measuring instrument 12 is abnormal, it can be filtered by the second filter. Therefore, the first filter 23a can be used for normal use and the second filter 23b can be used for abnormal use.
  • the second filter 23b is stopped after the abnormality by the fine particle measuring instrument 12 has been resolved, and the second filtration is performed.
  • the filtration membrane of the vessel 23b can be taken out and the fine particles captured on the filtration membrane can be analyzed.
  • the first filter 23a can be operated, and fine particles can be captured even during normal operation.
  • control of the 1st filter 23a and the 2nd filter 23b by the control part 24 can be performed by switching introduction of the sample water W with respect to each filter 23a, 23b, for example. More specifically, in each filter 23a, 23b, a switching valve (not shown) is provided in the piping 16 on the introduction side of the sample water W, and the control unit 24 controls the switching valve so that the first filtration is performed. It is possible to stop and operate the filter 23a and the second filter 23b.
  • FIG. 4 is a flowchart showing the fine particle measurement method of the present embodiment.
  • this flowchart figure also represents operation
  • FIG. 4 as a premise that the fine particle measurement method of the present embodiment is started, a state in which pure water W is introduced into the fine particle measurement device 12 and the first filter 23 a is started.
  • both the fine particle measuring instrument 12 and the first filter 23a are operated (step S21).
  • the particle measuring instrument 12 and the first filter 23a are not necessarily operated at the same time, and it is sufficient that both the particle measuring instrument 12 and the first filter 23a are in an operating state.
  • the rotation speed of the first filter (centrifugal filter) 23a, the filtration pressure, and one cycle of continuous operation depend on the target sample water, the place where the fine particle measurement method according to the present disclosure is applied, and the like. Can be set as appropriate.
  • the presence / absence of abnormality is confirmed in the measurement result by the particle measuring instrument 12 (step S22).
  • the presence or absence of this abnormality may be determined by the control unit 24 as described in the first embodiment, and the control unit 24 and the storage medium cooperate in the determination by the control unit 24.
  • You may comprise as follows. Similarly to the first embodiment, it is preferable that the control unit 24 determines that there is an abnormality when the fine particles are continuously measured for a predetermined number or more and for a predetermined time or more. Thereby, only the reliable abnormality resulting from the number and size of the fine particles by the fine particle measuring instrument 12 can be determined.
  • step S22 When abnormality is recognized by step S22, the 1st filter 23a is stopped and the 2nd filter 23b is operated (step S23). As a result, even when an abnormality is recognized by the particle measuring instrument 12, filtration is continuously performed.
  • the stop of the first filter 23a and the operation of the second filter 23b can be performed by controlling the first filter 23a and the second filter 23b by the control unit 24.
  • the rotation speed and filtration pressure of the second filter (second centrifugal filter) 23b can also be set as appropriate. From the viewpoint of continuing filtration from the first filter 23a, the first filter 23a and It is preferable to use the same conditions.
  • the second filter 23b is preferably operated immediately after the first filter 23a is stopped, and the stop of the first filter 23a is More preferably, the operation of the second filter 23b is performed at substantially the same timing. Since the first filter 23a and the second filter 23b are interlocked in this way, it is possible to suppress time loss, reduce the number of particles not captured (loss number), and increase the amount of captured particles.
  • step S22 Even if no abnormality is confirmed in step S22, the fine particle measuring instrument 12 and the first filter 23a remain in an operating state, and these are always in an operating state during normal operation (step S21).
  • the second filter 23b continuously operating is stopped after a predetermined time, and the first filter 23a is operated again (step S25).
  • the timing of stopping the second filter 23b is preferably when the abnormality is resolved in order to reliably capture the abnormal particles by the second filter 23b. In this case, it is preferable to determine whether or not the abnormality has been resolved in order to use the second filter 23b as a stop condition that the abnormality has been eliminated (step S24). This determination can also be performed by the control unit 24.
  • the timing for stopping the second filter 23b can be set after a predetermined time has elapsed after confirmation of the abnormality. The predetermined time is preferably set to a time sufficient for eliminating the abnormality, depending on the required water quality and the target sample water.
  • the filtration membrane is taken out from the second filter 23b, and the microparticles captured on the filtration membrane are directly examined by the microscopic method as in the method described in the first embodiment. Then, analysis and measurement of the number, size (particle size), composition, and the like of the fine particles are performed (step S26).
  • both the fine particle measuring device 12 and the first filter 23a are operated, and the measurement result of the fine particle measuring device 12 is abnormal.
  • the first filter 23a is stopped and the second filter 23b is operated, so that it is possible to capture fine particles in a timely manner in an abnormal state. Therefore, the number of fine particles that are not captured can be reduced, and the amount of captured fine particles can be increased.
  • the captured fine particles are analyzed in detail by a direct spectroscopic method, and it becomes possible to quickly investigate the cause of the abnormality in the measurement result by the fine particle measuring instrument 12, thereby improving the quality of fine particle management in pure water. It becomes possible.
  • the first filter 23a is always used and the second filter 23b is used for an abnormal time
  • the microparticles captured by the second filter 23b are directly analyzed by the microscopic method
  • the first filter 23a can be operated, and it is possible to constantly monitor fine particles in pure water.
  • FIG. 5 is a system diagram showing a configuration example for explaining the ultrapure water production facility 100 according to the present embodiment.
  • An ultrapure water production facility 100 described in the present embodiment includes a primary pure water production system 101 and an ultrapure water production system (also referred to as a subsystem and a secondary pure water production system) 102.
  • This ultrapure water production facility 100 is a facility for producing ultrapure water by further purifying the pure water produced by the primary pure water production system 101 using the ultrapure water production system 102.
  • the primary pure water production system (primary pure water production process) 101 is located in the previous stage of the ultra pure water production system (ultra pure water production process) 102, and sample water (pure water) W is supplied to the ultra pure water production system 102. It is a device for introduction.
  • the pre-stage of the primary pure water production system 101 usually has a pre-treatment device (pre-treatment process / not shown). In the pretreatment process, most of the suspended solids and part of the organic matter contained in the raw water (industrial water, city water, well water, etc.) to be treated are removed, and the load of the primary pure water production process in the subsequent stage Is performed.
  • the configuration of the pretreatment device is not particularly limited, and flocculation filtration, flocculation precipitation filtration, flocculation pressure flotation filtration, membrane filtration, and the like are used.
  • the configuration of the primary pure water production system 101 is also not particularly limited, and is a reverse osmosis (RO) membrane separation device, an ion exchange device, a desalination device, an adsorption device, an organic matter decomposition device (such as an ultraviolet oxidation device), and a deaeration Devices, sterilizers, etc. can be arranged in any order.
  • RO reverse osmosis
  • the ultrapure water production system (ultrapure water production process) 102 purifies the pure water W obtained in the primary pure water production process 101 to a higher purity, and generally includes a heat exchanger, ultraviolet oxidation. A device, an ion exchange device, an ultrafiltration device, and the like are combined.
  • the ultrapure water production system 102 of this embodiment receives the primary pure water W produced by the primary pure water production system 101 from the pipe 103a to the storage tank 104, draws it with the water supply pump 105, heat exchanger 106, low-pressure ultraviolet oxidizer. 107, deaeration device 108, ion exchange device 109, and ultrafiltration (UF) membrane device 110 are sequentially processed. And this ultrapure water manufacturing system 102 sends the ultrapure water obtained by each process to the use point 111 by the piping 103b, and returns surplus water to the storage tank 104 by the piping 103c.
  • the ultrapure water production system 102 is provided with the particulate measurement system 31 of the present disclosure.
  • the installation location of the particulate measurement system 31 in the ultrapure water production system 102 is not particularly limited.
  • a particulate measurement system 21 is provided by branching a pipe 103b through which treated water (ultra pure water) of the UF membrane device 110 passes after the UF membrane device 110 in the ultra pure water production system 102. . Then, the treated water (ultra pure water) of the UF membrane device 110 is configured to be introduced into the fine particle measurement system 31.
  • the fine particle measurement system 31 includes a fine particle measuring instrument (measuring unit) 32, filters (filtering units) 33a and 33b, and a control unit (not shown).
  • a fine particle measuring instrument measuring unit
  • filters filtering units
  • control unit not shown
  • the filters 33a and 33b the first centrifugal filter 33a and the second centrifugal filter 33b applicable to the fine particle measurement method and the fine particle measurement system of the second embodiment can be used.
  • the operations of the first filter 33a and the second filter 33b are the same as those described in the second embodiment.
  • the second filter 33b should be removed. That's fine.
  • first separation membrane unit 33c and second separation membrane unit 33d can also be used (shown in parentheses in FIG. 5).
  • on-off valves 331 and 332 can switch between the stop and operation of filtration by the separation membrane units 33c and 33d. In this case, the first separation membrane unit 33c is always used for operation, and the second separation membrane unit 33d is used for abnormal operation.
  • the first on-off valve 331 at the rear stage of the first separation membrane unit 33c is opened.
  • the second on-off valve 332 at the rear stage of the second separation membrane unit 33d in the stopped state is opened from the closed state.
  • Both the first on-off valve 331 and the second on-off valve 332 can be controlled by a control unit (not shown), and the control unit cooperates with the fine particle measuring device 32 to provide the first on-off valve 331 and the second on-off valve 332.
  • the two on-off valve 332 can be opened and closed automatically.
  • the ultrapure water production system 102 (ultrapure water production facility 100) of the third embodiment, since the fine particle measurement system 31 according to the present disclosure is provided, the effects of the fine particle measurement system 31 are provided. Can play. In addition, since the fine particle measurement system 31 can capture the fine particles in a timely manner, it is possible to further improve the quality (quality) of the manufactured ultrapure water. Therefore, the ultrapure water production system 102 of the present embodiment is suitably used in various industrial fields such as the semiconductor manufacturing field and the pharmaceutical manufacturing field.
  • the fine particle measurement method and the fine particle measurement system of the present disclosure can be configured as follows.
  • various parts such as a dissolved gas concentration meter, a TOC meter, a hydrogen peroxide concentration meter, a silica meter, a boron meter, an evaporation residue meter, and a water temperature meter are used as a unit for monitoring water quality. It is also possible to provide a measuring instrument.
  • the structure provided with two filters was illustrated, the number of filters is good also as 2 or more. In this case, it is preferable to provide a control unit capable of controlling each filter.
  • the present invention can also employ the following configurations.
  • the measurement unit that measures the fine particles in the sample water and the filtration unit that filters the sample water and captures the fine particles for direct spectroscopic analysis are operated together to measure the measurement unit.
  • the filtration unit includes a first filtration unit and a second filtration unit that are installed so that the supply of the sample water can be switched, and the measurement unit and the first filtration unit are both operating.
  • the fine particle measurement system wherein the control unit continuously operates the filtration unit even when an abnormality is found in the measurement result by the measurement unit.
  • the filtration unit includes a first filtration unit and a second filtration unit that are installed so that the supply of the pure water can be switched, and the control unit includes the measurement unit and the first filtration unit.
  • the particulate measurement system according to [8] above, wherein when the abnormality is recognized in the measurement result by the measurement unit in a state where both are operating, the first filtration unit is stopped and the second filtration unit is operated. .
  • the control unit stops the filtering unit that is continuously filtered after an abnormality is recognized in the measurement result by the measuring unit, after the abnormality is resolved, ] The fine particle measuring system according to any one of the above.
  • the control unit may determine that the abnormality is detected when the measurement unit continuously measures the fine particles for a predetermined number or more and for a predetermined time. The particulate measurement system described.
  • An ultrapure water production system comprising the fine particle measurement system according to any one of [8] to [12] in an ultrapure water production process.

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Abstract

To provide a technology whereby particulates in a water sample can still be trapped in a timely manner even in a state in which an anomaly has been found in measurement results from a measurement unit that measures the particulates in the water sample. The following process is performed in the provided particulate-measuring method: a measurement unit that measures particulates in a water sample and a filtration unit that filters said water sample and traps the particulates for analysis via direct microscopic counting are both run, and even if an anomaly is found in measurement results from the measurement unit, filtration of the water sample is continued.

Description

微粒子測定方法及び微粒子測定システム並びに超純水製造システムFine particle measurement method, fine particle measurement system, and ultrapure water production system
　本発明は、試料水中の微粒子の測定に用いられる微粒子測定方法及び微粒子測定システムに関する。 The present invention relates to a fine particle measurement method and a fine particle measurement system used for measuring fine particles in sample water.
　従来から、純水（超純水を含む）は、半導体製造分野及び医薬品製造分野等の様々な工業分野において使用されている。工業分野で使用される純水の水質に対する要求は近年高まっており、一次純水製造装置や超純水製造設備等において、要求水質が維持されていることを確認するための検査及び管理が行われている。こうした検査及び管理において、水質管理項目の一つとして、純水１ｍｌ中に含まれる微粒子の数が挙げられている。 Conventionally, pure water (including ultrapure water) has been used in various industrial fields such as the semiconductor manufacturing field and the pharmaceutical manufacturing field. The demand for the quality of pure water used in the industrial field has been increasing in recent years, and inspection and management are performed to confirm that the required water quality is maintained in primary pure water production equipment and ultrapure water production facilities. It has been broken. In such inspection and management, one of the water quality management items is the number of fine particles contained in 1 ml of pure water.
　純水中の微粒子の管理方法としては、一般的に、日常の微粒子管理として、オンライン式の微粒子カウンターにて、純水中の微粒子数の測定及び監視が行われている。例えば、特許文献１には、微粒子数を計測する微粒子計、ＴＯＣ（全有機体炭素量）値を計測するＴＯＣ計、及び比抵抗値を計測する比抵抗計等を備える超純水製造装置が開示されている。 As a method for managing fine particles in pure water, the number of fine particles in pure water is generally measured and monitored by an online fine particle counter as a daily fine particle management. For example, Patent Document 1 discloses an ultrapure water production apparatus including a fine particle meter that measures the number of fine particles, a TOC meter that measures a TOC (total organic carbon content) value, a specific resistance meter that measures a specific resistance value, and the like. It is disclosed.
　また、特許文献２には、超純水中の微粒子数を測定する方法及び装置として、超純水をフィルタで濾過し、そのフィルタに付着した微粒子数を顕微鏡で計数するものが記載されている。この微粒子数の測定方法は、直接検鏡法と称され、通常、定期的な検査時又は異常時等に、微粒子の詳細な分析を行うために用いられている。 Patent Document 2 describes a method and apparatus for measuring the number of fine particles in ultrapure water by filtering ultrapure water with a filter and counting the number of fine particles adhering to the filter with a microscope. . This method of measuring the number of fine particles is called a direct spectroscopic method, and is usually used for performing a detailed analysis of fine particles during periodic inspections or abnormal times.
特開平５－１３８１９６号公報JP-A-5-138196 特開平１０－６３８１０号公報JP 10-63810 A
　オンライン式の微粒子カウンターでは、純水中の微粒子を簡易にオンタイムで測定できるという利点があり、この利点から、純水中の微粒子数をモニタリングするという、日常の微粒子管理が行われている。しかし、オンライン式の微粒子カウンターでは、微粒子の粒径が小さい程、リアルタイムでの測定が困難となり、高まる要求水質に対して満足な測定が困難となる。
　直接検鏡法では、詳細な分析が可能であり、要求水質に対して満足する測定が可能であるが、リアルタイムでの測定はできず、分析に時間を要する。そのため、直接検鏡法は、上述のとおり、定期的検査時、又は上記微粒子計にて所定数以上の微粒子が計測される等の異常が確認された場合に限って用いることが常識的に考えられている。 The on-line particle counter has the advantage that it can easily measure the fine particles in pure water on-time, and from this advantage, daily particle management is performed to monitor the number of fine particles in pure water. However, in the on-line type fine particle counter, the smaller the particle size of the fine particles, the more difficult the measurement in real time becomes, and the more difficult the measurement is with respect to the increasing required water quality.
In the direct spectroscopic method, detailed analysis is possible and measurement that satisfies the required water quality is possible, but real-time measurement is not possible and analysis takes time. For this reason, as described above, it is common sense that the direct spectroscopic method is used only during periodic inspections or when abnormalities such as measurement of a predetermined number or more of particles are confirmed by the particle counter. It has been.
　しかしながら、異常時が認められた後に、直接検鏡法のための濾過を行うとなると、微粒子ハンチング（乱調）が生じている間にタイムリーに微粒子を捕捉できない可能性がある。これは、濾過膜の交換作業時や、定期的検査における定期検査時と定期検査時の間に、微粒子数にハンチングが生じた場合に、タイムロスにより、微粒子の捕捉量が少なくなることに起因する。また、ハンチングが微粒子によるものか単なる微粒子計測器の一時的な異常であるかを判断するため、通常、ハンチングが生じてもすぐに回復する場合は、異常なしと判断でき、実際に異常があったときには捕捉のタイミングを逸してしまうおそれが生じる。 However, if filtration for direct microscopic examination is performed after an abnormal time is recognized, there is a possibility that the particles cannot be captured in a timely manner while the particle hunting (disturbance) is occurring. This is because, when hunting occurs in the number of fine particles during the replacement work of the filtration membrane or during the periodic inspection in the periodic inspection, the amount of captured fine particles is reduced due to time loss. In addition, in order to determine whether hunting is caused by fine particles or just a temporary abnormality of the particle measuring instrument, if it recovers immediately even if hunting occurs, it can be determined that there is no abnormality and there is actually an abnormality. If this happens, the capture timing may be lost.
　そこで、本発明は、試料水中の微粒子を測定する計測部による測定結果に異常が認められた状況においても、タイムリーに試料水中の微粒子を捕捉することができる微粒子測定方法及び微粒子測定システムを提供することを主目的とする。 Therefore, the present invention provides a fine particle measurement method and a fine particle measurement system that can capture fine particles in sample water in a timely manner even in a situation where an abnormality is recognized in the measurement result by the measurement unit that measures the fine particles in sample water. The main purpose is to do.
　本発明は、試料水中の微粒子を測定する計測部と、前記試料水を濾過し、前記微粒子を直接検鏡法による分析用に捕捉する濾過部と、を共に稼働させておき、前記計測部の測定結果に異常が認められた場合にも、継続して前記試料水を濾過する工程を行う、微粒子測定方法を提供する。
　本発明の微粒子測定方法は、計測部と、直接検鏡法による分析用の濾過部とを共に稼働させておき、計測部の測定結果に異常が認められた場合にも継続して試料水の濾過を行うため、異常時でもタイムリーに微粒子を捕捉することが可能となる。
　本発明の微粒子測定方法では、前記計測部の測定結果に異常が認められた場合にも、前記濾過部を継続して稼働させることで、継続して前記試料水を濾過する工程を行うことができる。
　また、本発明の微粒子測定方法では、前記濾過部は、前記試料水の供給を切り替え可能に設置された第１濾過部と第２濾過部とを有し、前記計測部と前記第１濾過部とが共に稼働している状態で、前記計測部による測定結果に異常が認められた場合に、前記第１濾過部を停止すると共に、前記第２濾過部を稼働させることで、継続して前記試料水をろ過する工程を行うことができる。
　本発明の微粒子測定方法では、前記計測部による測定結果に異常が認められた後に継続して濾過が行われている濾過部を、前記異常が解消した後に停止することができる。そして、前記計測部による測定結果に異常が認められた後に継続して濾過が行われている濾過部により捕捉された微粒子の分析を行うことができる。この際の微粒子の分析は、光学顕微鏡又は走査型電子顕微鏡を用いて測定する、いわゆる直接検鏡法にて行うことができる。 The present invention operates both a measurement unit that measures fine particles in sample water and a filtration unit that filters the sample water and captures the fine particles for direct spectroscopic analysis. Provided is a fine particle measurement method in which even when an abnormality is found in a measurement result, the step of continuously filtering the sample water is performed.
In the method for measuring fine particles of the present invention, the measurement unit and the filtration unit for analysis by the direct spectroscopic method are operated together, and even if an abnormality is recognized in the measurement result of the measurement unit, the sample water is continued. Since filtration is performed, it becomes possible to capture fine particles in a timely manner even when an abnormality occurs.
In the fine particle measurement method of the present invention, even when an abnormality is found in the measurement result of the measurement unit, the step of continuously filtering the sample water can be performed by continuously operating the filtration unit. it can.
In the fine particle measurement method of the present invention, the filtration unit includes a first filtration unit and a second filtration unit that are installed so that the supply of the sample water can be switched, and the measurement unit and the first filtration unit. In the state where both are in operation, when an abnormality is recognized in the measurement result by the measurement unit, the first filtration unit is stopped and the second filtration unit is operated, thereby continuously A step of filtering the sample water can be performed.
In the fine particle measurement method of the present invention, the filtration unit that is continuously filtered after an abnormality is recognized in the measurement result by the measurement unit can be stopped after the abnormality is resolved. Then, it is possible to analyze the fine particles captured by the filtration unit that is continuously filtered after an abnormality is recognized in the measurement result by the measurement unit. In this case, the analysis of the fine particles can be performed by a so-called direct spectroscopic method in which measurement is performed using an optical microscope or a scanning electron microscope.
　また、本発明は、試料水中の微粒子を測定する計測部と、前記試料水を濾過し、前記微粒子を直接検鏡法による分析用に捕捉する濾過部と、前記計測部及び前記濾過部が共に稼働している状態で、前記計測部による測定結果に異常が認められた場合に、前記試料水の濾過が継続して行われるように制御する制御部と、を備える、微粒子測定システムを提供する。
　前記制御部は、前記計測部による測定結果に異常が認められた場合にも、前記濾過部を継続して稼働させることができる。
　前記濾過部は、前記試料水の供給を切り替え可能に設置された第１濾過部と第２濾過部とを有し、前記制御部は、前記計測部と前記第１濾過部とが共に稼働している状態で、前記計測部による測定結果に異常が認められた場合に、前記第１濾過部を停止すると共に前記第２濾過部を稼働させることができる。
　前記制御部は、前記計測部による測定結果に異常が認められた後に継続して濾過が行われている濾過部を、前記異常が解消した後に停止することができる。
　前記制御部は、前記計測部によって、前記微粒子が所定数以上かつ所定時間連続して測定された場合に前記異常と判定することができる。 The present invention also includes a measuring unit that measures fine particles in sample water, a filtering unit that filters the sample water and captures the fine particles for analysis by direct spectroscopic method, and both the measuring unit and the filtering unit. Provided is a fine particle measurement system comprising: a control unit that performs control so that the sample water is continuously filtered when an abnormality is found in the measurement result of the measurement unit in an operating state. .
The control unit can continuously operate the filtering unit even when an abnormality is recognized in the measurement result by the measuring unit.
The filtration unit includes a first filtration unit and a second filtration unit that are installed so that the supply of the sample water can be switched, and the control unit operates with both the measurement unit and the first filtration unit. When the abnormality is recognized in the measurement result by the measurement unit, the first filtration unit can be stopped and the second filtration unit can be operated.
The said control part can stop the filtration part currently filtered after abnormality is recognized by the measurement part by the said measurement part, after the said abnormality is eliminated.
The control unit can determine that the abnormality is detected when the measurement unit continuously measures the fine particles for a predetermined number or more and for a predetermined time.
　さらに、本発明は、上記本発明に係る微粒子測定システムを純水の製造工程に備える超純水製造システムを提供する。 Furthermore, the present invention provides an ultrapure water production system comprising the fine particle measurement system according to the present invention in a pure water production process.
　本発明によれば、試料水中の微粒子を測定する計測部の測定結果に異常が認められた状況においても、タイムリーに試料水中の微粒子を捕捉することができる微粒子測定方法及び微粒子測定システムが提供される。 According to the present invention, there are provided a fine particle measurement method and a fine particle measurement system capable of capturing fine particles in a sample water in a timely manner even in a situation where an abnormality is found in the measurement result of the measurement unit that measures the fine particles in the sample water. Is done.
本発明の第１実施形態の微粒子測定方法を適用した微粒子測定システムの一構成例を示す系統図である。1 is a system diagram showing an example of the configuration of a particle measuring system to which a particle measuring method according to a first embodiment of the present invention is applied. 本発明の第１実施形態の微粒子測定方法を表すフローチャート図である。It is a flowchart figure showing the particulate measuring method of a 1st embodiment of the present invention. 本発明の第２実施形態の微粒子測定方法を適用した微粒子測定システムの一構成例を示す系統図である。It is a systematic diagram which shows the example of 1 structure of the fine particle measurement system to which the fine particle measurement method of 2nd Embodiment of this invention is applied. 本発明の第２実施形態の微粒子測定方法を表すフローチャート図である。It is a flowchart figure showing the particulate measuring method of a 2nd embodiment of the present invention. 本発明の微粒子測定システムを適用した超純水製造設備の構成例を示す系統図である。It is a systematic diagram which shows the structural example of the ultrapure water manufacturing equipment to which the fine particle measurement system of this invention is applied.
　以下、本発明を実施するための形態について、詳細に説明する。なお、本発明は、以下に説明する実施形態に限定されるものではない。 Hereinafter, embodiments for carrying out the present invention will be described in detail. Note that the present invention is not limited to the embodiments described below.
　本開示に係る微粒子測定方法は、試料水中の微粒子を測定する計測部と、試料水を濾過し、微粒子を直接検鏡法による分析用に捕捉する濾過部と、を共に稼働させておき、計測部による測定結果に異常が認められた場合にも、継続して上記試料水を濾過する工程を行うものである。 The fine particle measurement method according to the present disclosure includes a measurement unit that measures fine particles in sample water, and a filtration unit that filters the sample water and captures the fine particles for analysis by direct microscopic analysis. The process of continuously filtering the sample water is performed even when an abnormality is found in the measurement result by the section.
　本開示に係る微粒子測定方法では、上記計測部と、上記濾過部とを共に稼働状態としておき、計測部の測定結果に異常が認められた場合にも継続して試料水を濾過する工程が行われる。そのため、計測部による測定結果の異常時にもタイムリーに試料水中の微粒子を捕捉することができる。また、タイムリーに微粒子を捕捉できることから、捕捉されない微粒子数（ロス数）を抑え、微粒子の捕捉量を多くすることが可能となる。そして、捕捉された微粒子を直接検鏡法にて詳細に分析することが可能となる。よって、本開示に係る微粒子測定方法では、計測部による測定結果の異常原因を迅速に特定することに繋がり、純水中の微粒子管理の質を向上することが可能となる。 In the fine particle measurement method according to the present disclosure, the step of continuously filtering the sample water is performed even when the measurement unit and the filtration unit are both in an operating state and an abnormality is recognized in the measurement result of the measurement unit. Is called. Therefore, it is possible to capture fine particles in the sample water in a timely manner even when the measurement result by the measurement unit is abnormal. In addition, since the fine particles can be captured in a timely manner, the number of fine particles that are not captured (the number of losses) can be suppressed, and the amount of captured fine particles can be increased. The captured fine particles can be analyzed in detail by direct spectroscopic methods. Therefore, in the fine particle measurement method according to the present disclosure, it is possible to quickly identify the cause of the abnormality in the measurement result by the measurement unit, and it is possible to improve the quality of fine particle management in pure water.
　本開示の微粒子測定方法は、当該方法における工程（手順）を、例えば、測定される微粒子の大きさ（粒径）及び数等を管理するための装置（例えば、パーソナルコンピュータ等）のＣＰＵ等を含む制御部、及び記憶媒体（ＵＳＢメモリ、ＨＤＤ、ＣＤ等）等を備えるハードウエア資源にプログラムとして格納し、制御部によって実現させることも可能である。 The fine particle measurement method of the present disclosure includes a process (procedure) in the method, for example, a CPU of an apparatus (for example, a personal computer or the like) for managing the size (particle diameter) and the number of fine particles to be measured. It is also possible to store it as a program in a hardware resource including a control unit and a storage medium (USB memory, HDD, CD, etc.) and realize the program by the control unit.
　本開示の微粒子測定方法は、制御部を備えた微粒子測定システムに適用して実行することができる。
　この微粒子測定システムは、試料水中の微粒子を測定する計測部と、試料水を濾過し、微粒子を直接検鏡法による分析用に捕捉する濾過部とが共に稼働している状態で、計測部による測定結果に異常が認められた場合に、試料水の濾過が継続して行われるように制御する制御部と、を備えて構成することができる。 The fine particle measurement method of the present disclosure can be executed by being applied to a fine particle measurement system including a control unit.
This fine particle measurement system is operated by a measurement unit in a state where a measurement unit that measures fine particles in sample water and a filtration unit that filters sample water and captures the fine particles for direct spectroscopic analysis are in operation. And a control unit that controls the sample water to be continuously filtered when an abnormality is found in the measurement result.
　本開示の微粒子測定方法及び微粒子測定システムは、一次純水製造システムに適用することができ、より好適には、一次純水製造システムにて製造された純水をさらに精製処理する超純水製造システム（二次純水製造システム及びサブシステムとも称される。）に適用することができる。
　一次純水製造システムは、純水に仕上げる装置であり、例えば、イオン交換樹脂、逆浸透膜、又はこれらを組み合わせたものなどが挙げられる。
　二次純水製造システムは、例えば、熱交換器、紫外線酸化装置、イオン交換装置、及び限外濾過装置等を組み合わせて構成される。 The fine particle measurement method and the fine particle measurement system of the present disclosure can be applied to a primary pure water production system, and more preferably, ultrapure water production that further purifies pure water produced by the primary pure water production system. It can be applied to a system (also referred to as a secondary pure water production system and a subsystem).
The primary pure water production system is an apparatus for finishing to pure water, and examples thereof include an ion exchange resin, a reverse osmosis membrane, or a combination thereof.
The secondary pure water production system is configured by combining, for example, a heat exchanger, an ultraviolet oxidation device, an ion exchange device, and an ultrafiltration device.
　本開示の微粒子測定方法及び微粒子測定システムの対象となる試料水は、特に限定されるものではなく、例えば、一次純水製造システムの製造工程における純水、及び二次純水製造システムの超純水の製造工程における超純水が挙げられる。また、「試料水」には、上記純水及び超純水のほか、イオン成分、有機物及び微粒子等の不純物を除去する対象となる水が含まれるものとする。 The sample water that is the target of the fine particle measurement method and the fine particle measurement system of the present disclosure is not particularly limited. For example, the pure water in the production process of the primary pure water production system and the ultrapure of the secondary pure water production system Examples include ultrapure water in the water production process. In addition to the pure water and ultrapure water, the “sample water” includes water that is a target for removing impurities such as ionic components, organic substances, and fine particles.
　本開示の微粒子測定方法及び微粒子測定システムについて、以下の第１～３実施形態でより詳細に説明する。 The fine particle measurement method and the fine particle measurement system of the present disclosure will be described in more detail in the following first to third embodiments.
＜第１実施形態＞
　第１実施形態に係る微粒子測定方法は、上記計測部として微粒子計測器と、上記濾過部として濾過器とを共に稼働させておき、微粒子計測器の測定結果に異常が認められた場合にも、濾過器を継続して稼働させることで、濾過を継続して行うものである。 <First Embodiment>
In the fine particle measurement method according to the first embodiment, both the fine particle measuring instrument as the measuring unit and the filter as the filtering unit are operated together, and even when an abnormality is recognized in the measurement result of the fine particle measuring instrument, By continuously operating the filter, the filtration is continuously performed.
　図１は、本実施形態の微粒子測定方法を適用した微粒子測定システムの一構成例（第１実施形態に係る微粒子測定システム）を示す系統図である。
　本実施形態の微粒子測定システム１１は、微粒子計測器１２、濾過器１３、及び制御部１４を備える。本実施形態では、微粒子計測器１２及び濾過器１３は、貯槽１５に貯留された試料水（本実施形態では純水）Ｗが流れる配管１６から分岐して接続されている。 FIG. 1 is a system diagram showing a configuration example (a fine particle measurement system according to the first embodiment) of a fine particle measurement system to which the fine particle measurement method of the present embodiment is applied.
The fine particle measurement system 11 according to the present embodiment includes a fine particle measurement device 12, a filter 13, and a control unit 14. In the present embodiment, the particle measuring instrument 12 and the filter 13 are branched and connected from a pipe 16 through which sample water (pure water in the present embodiment) W stored in the storage tank 15 flows.
　微粒子計測器１２としては、市販のレーザー散乱光等を用いたオンライン式の光散乱式微粒子自動計測器が好適である。
　この微粒子計測器１２は、配管１６から純水Ｗが導入されて、少なくとも、純水中の微粒子の数が測定される。本実施形態の微粒子計測器１２は、純水中の微粒子の数及び大きさ（粒径）を連続的に測定することが可能である。この微粒子計測器１２によって、ＪＩＳ　Ｋ０５５４（超純水中の微粒子測定方法）における「微粒子自動計測器による測定方法」に準拠した微粒子の測定が行われる。 As the fine particle measuring device 12, an on-line light scattering fine particle automatic measuring device using commercially available laser scattered light or the like is suitable.
The fine particle measuring instrument 12 receives pure water W from the pipe 16 and measures at least the number of fine particles in the pure water. The fine particle measuring instrument 12 of the present embodiment can continuously measure the number and size (particle size) of fine particles in pure water. The fine particle measuring device 12 measures fine particles in accordance with “Measurement method using automatic fine particle measuring device” in JIS K0554 (fine particle measuring method in ultrapure water).
　微粒子計測器１２は、単位体積当たりの水中の微粒子数（単位：個／ｍｌ）を測定値としてモニタに出力し、常時、オンタイム（リアルタイム）で純水中の微粒子数を測定し、監視する。そして、微粒子計測器１２により、測定結果である微粒子数に異常が認められたか否かが確認される。 The fine particle measuring device 12 outputs the number of fine particles in water per unit volume (unit: piece / ml) to the monitor as a measurement value, and always measures and monitors the number of fine particles in pure water on time (real time). . Then, the particle measuring instrument 12 confirms whether or not an abnormality is recognized in the number of particles as a measurement result.
　微粒子計測器１２による測定結果における「異常」は、要求水質に応じて、測定された微粒子の粒径及び数、並びに確認された時間等から設定される。
　例えば、微粒子計測器１２により、所定数以上の微粒子が所定時間以上確認された場合を「異常」と設定することができる。微粒子計測器１２により測定される微粒子の上記「所定数」としては、例えば、１００～１００００個／Ｌ（好適には５００～５０００個／Ｌ）の範囲から設定することができる。同様に、上記「所定時間」としては、例えば、３０秒～３０分（好適には１分～１０分）の範囲で設定することができる。これらの範囲において、超純水製造システムで好適に設定され得る一具体例を挙げると、微粒子計測器１２により、例えば１０００個／Ｌ以上の微粒子が連続で５分間以上確認された場合に、「異常」と設定することができる。 The “abnormality” in the measurement result by the particle measuring instrument 12 is set from the particle diameter and number of the measured particles, the confirmed time, and the like according to the required water quality.
For example, a case where a predetermined number of fine particles or more are confirmed by a fine particle measuring instrument 12 for a predetermined time or more can be set as “abnormal”. The “predetermined number” of fine particles measured by the fine particle measuring instrument 12 can be set, for example, from a range of 100 to 10,000 / L (preferably 500 to 5000 / L). Similarly, the “predetermined time” can be set, for example, in the range of 30 seconds to 30 minutes (preferably 1 minute to 10 minutes). In these ranges, one specific example that can be suitably set in the ultrapure water production system is as follows. For example, when the fine particle measuring device 12 continuously confirms, for example, 1000 particles / L or more fine particles for 5 minutes or more, “ “Abnormal” can be set.
　濾過器１３は、配管１６から導入された純水Ｗを濾過し、直接検鏡法による分析用に微粒子を捕捉するものであり、微粒子を捕捉するための濾過膜を備える。この濾過器１３は、微粒子計測器１２で測定困難なほど小さい粒子径の微粒子についても、濾過膜で微粒子を捕捉し、直接検鏡法にて分析するためのものである。直接検鏡法では、例えば、微粒子の大きさ（粒径）、数、及び組成等を分析することができる。 The filter 13 filters the pure water W introduced from the pipe 16 and captures fine particles for analysis by a direct spectroscopic method, and includes a filtration membrane for capturing the fine particles. The filter 13 is for capturing fine particles with a filtration membrane and analyzing them directly by a microscopic method even for fine particles having such a small particle diameter that it is difficult to measure with the fine particle measuring instrument 12. In the direct microscopic method, for example, the size (particle diameter), number, composition, and the like of fine particles can be analyzed.
　濾過器１３としては、純水Ｗ中の微粒子を濾過膜に捕捉できれば特に限定されるものではない。そのような濾過器１３としては、遠心濾過器、及び通水圧（給水圧）を用いた分離膜ユニットを用いることができる。
　通水圧を用いた分離膜ユニットは、分離膜（濾過膜）を有し、濾過の動力が通水圧による構造とされたユニットである。濾過の動力が通水圧によることから必要な濾過水量を稼ぐために通水に時間を要するものの、簡易に設置できることから好適である。
　遠心濾過器は、濾過に遠心力を用いるため、通水圧を用いた分離膜ユニットに比べて、短時間で必要な濾過水量を稼ぐことが可能であることからより好適である。本実施形態では、濾過器１３として遠心濾過器１３を用いている。 The filter 13 is not particularly limited as long as the fine particles in the pure water W can be captured by the filtration membrane. As such a filter 13, a centrifugal filter and a separation membrane unit using a water pressure (feed water pressure) can be used.
The separation membrane unit using the water passage pressure is a unit having a separation membrane (filtration membrane) and having a structure in which the power of filtration is based on the water passage pressure. Since the power of filtration depends on the water flow pressure, it takes time to pass the water in order to earn the necessary amount of filtered water, but it is preferable because it can be easily installed.
Since the centrifugal filter uses centrifugal force for filtration, the centrifugal filter is more preferable because a necessary amount of filtered water can be obtained in a shorter time than a separation membrane unit using a water flow pressure. In the present embodiment, the centrifugal filter 13 is used as the filter 13.
　本開示の微粒子測定方法及び微粒子測定システム１１で用いられる濾過器１３による濾過時間は、特に限定されず、要求水質に応じて適宜設定される。
　例えば、要求水質として、粒径０．０５μｍ以上の微粒子１個／ｍｌを測定する場合、遠心濾過器では、圧力２ＭＰａで２０日以上が望ましく、通水圧による濾過では、圧力０．４ＭＰａと設定した場合で１００日以上が望ましい。
　なお、上記濾過時間は、濾過器１３に用いられる濾過膜の製膜時のブランク数値、顕微鏡観察による分析時の観察視野数、対象粒径及び想定される微粒子濃度等により、変動される。 The filtration time by the filter 13 used in the fine particle measurement method and the fine particle measurement system 11 of the present disclosure is not particularly limited, and is appropriately set according to the required water quality.
For example, when measuring 1 minute / ml of particles having a particle size of 0.05 μm or more as the required water quality, it is desirable that the centrifugal filter has a pressure of 2 MPa and 20 days or more, and the filtration by water pressure sets the pressure to 0.4 MPa. In some cases, 100 days or more is desirable.
In addition, the said filtration time is fluctuate | varied with the blank numerical value at the time of film-forming of the filter membrane used for the filter 13, the number of observation visual fields at the time of the analysis by microscopic observation, a target particle size, assumed fine particle concentration, etc.
　濾過器１３に用いられる濾過膜は、通常の純水製造分野において用いられている市販品を用いることができる。濾過膜は、測定しようとする微粒子を表面に捕捉することができ、かつ試料水を通水できるような構造を有していれば特に限定されない。
　例えば、濾過膜の孔径別の種類としては、精密濾過膜（ＭＦ膜）、限外濾過膜（ＵＦ膜）、及び逆浸透膜（ＲＯ膜）等が挙げられる。濾過膜の構造としては、例えば、中空糸膜、スパイラル膜、及びチューブラー膜等が挙げられる。濾過膜の材質としては、例えば、酢酸セルロース、芳香族ポリアミド、ポリビニルアルコール、ポリフッ化ビニリデン、ポリエチレン、ポリアクリロニトリル、ポリプロピレン、ポリカーボネート、ポリテトラフルオロエチレン、及びセラミック等が挙げられる。 The filtration membrane used for the filter 13 can use the commercial item used in the normal pure water manufacture field | area. The filtration membrane is not particularly limited as long as it has a structure capable of capturing fine particles to be measured on the surface and allowing sample water to pass therethrough.
For example, the types of filtration membranes by pore size include microfiltration membranes (MF membranes), ultrafiltration membranes (UF membranes), and reverse osmosis membranes (RO membranes). Examples of the structure of the filtration membrane include a hollow fiber membrane, a spiral membrane, and a tubular membrane. Examples of the material of the filtration membrane include cellulose acetate, aromatic polyamide, polyvinyl alcohol, polyvinylidene fluoride, polyethylene, polyacrylonitrile, polypropylene, polycarbonate, polytetrafluoroethylene, and ceramic.
　制御部１４は、少なくとも濾過器１３を制御する機能を有する。そして、制御部１４は、微粒子計測器１２と濾過器１３とが共に稼働している状態において、微粒子計測器１２による測定結果に異常が認められた場合にも、濾過器１３を継続して稼働させて、純水の濾過が継続して行われるように制御する部である。制御部１４は、濾過器１３に備わっていてもよく、濾過器１３とは別途、設けられていてもよい。 The control unit 14 has a function of controlling at least the filter 13. The control unit 14 continues to operate the filter 13 even when an abnormality is found in the measurement result by the particle measuring instrument 12 in a state where both the particle measuring instrument 12 and the filter 13 are operating. It is a part which controls so that filtration of pure water may be performed continuously. The control unit 14 may be provided in the filter 13 or may be provided separately from the filter 13.
　また、制御部１４は、濾過器１３のほか、微粒子計測器１２を制御する機能を有していてもよい。例えば、微粒子計測器１２と制御部１４とが協働し、微粒子計測器１２による測定結果が制御部１４へ出力され、制御部１４が当該測定結果を異常か否か判定するように構成してもよい。
　制御部１４による異常の有無の判定には、例えば、制御部１４と協働する記憶媒体に測定結果の正常値及び異常値を記憶させておき、制御部１４が記憶媒体に記憶された、測定結果の正常値及び異常値のデータに基づき、判定することができる。
　また、微粒子計測器１２による測定結果の異常がすぐに解消する場合や、微粒子計測器１２自体の不具合による異常が確認される場合を考慮して、制御部１４は、微粒子が所定数以上かつ所定時間以上連続して測定された場合に異常と判定することが好ましい。これにより、微粒子計測器１２による微粒子の数及び大きさ等に起因する確実な異常のみを判定することができる。ここで「所定数」及び「所定時間」は、上述した微粒子計測器１２による測定結果における「異常」で説明した範囲で設定することができる。なお、後記の「所定数」及び「所定時間」についても同様である。 Further, the control unit 14 may have a function of controlling the particle measuring instrument 12 in addition to the filter 13. For example, the particle measuring instrument 12 and the control unit 14 cooperate to output a measurement result by the particle measuring instrument 12 to the control unit 14, and the control unit 14 determines whether or not the measurement result is abnormal. Also good.
For the determination of the presence or absence of abnormality by the control unit 14, for example, the normal value and the abnormal value of the measurement result are stored in a storage medium cooperating with the control unit 14, and the control unit 14 stores the measurement value in the storage medium. The determination can be made based on the normal value and abnormal value data of the result.
Further, in consideration of the case where the abnormality of the measurement result by the particle measuring instrument 12 is resolved immediately or the case where the abnormality due to the defect of the particle measuring instrument 12 itself is confirmed, the control unit 14 has a predetermined number or more of the particles. It is preferable to determine that there is an abnormality when measured continuously for more than a time. Thereby, only the reliable abnormality resulting from the number and size of the fine particles by the fine particle measuring instrument 12 can be determined. Here, the “predetermined number” and the “predetermined time” can be set within the range described in the “abnormality” in the measurement result by the fine particle measuring instrument 12 described above. The same applies to “predetermined number” and “predetermined time” described later.
　図２は、本実施形態の微粒子測定方法を表すフローチャート図である。なお、このフローチャート図は、上述の本実施形態の微粒子測定システム１１の動作も表している。
　図２では、本実施形態の微粒子測定方法が開始される前提として、微粒子計測器１２及び濾過器１３に純水Ｗが導入されている状態をスタートとしている。 FIG. 2 is a flowchart showing the fine particle measurement method of the present embodiment. In addition, this flowchart figure also represents operation | movement of the particulate measuring system 11 of this embodiment mentioned above.
In FIG. 2, as a premise that the fine particle measurement method of the present embodiment is started, a state where pure water W is introduced into the fine particle measuring instrument 12 and the filter 13 is started.
　本実施形態の微粒子測定方法では、微粒子計測器１２及び濾過器１３の両方を稼働させておく（ステップＳ１１）。微粒子計測器１２と濾過器１３とは必ずしも同時に稼働させる必要はなく、微粒子計測器１２と濾過器１３とが共に稼働状態にあればよい。
　ここで、微粒子計測器の稼働状態とは、微粒子計測器に試料水が導入され、微粒子計測器により、試料水中に含まれる微粒子の測定が行われている状態をいう。また、濾過器の稼働状態とは、濾過器に純水が導入され、試料水の濾過が行われている状態をいう。このとき、試料水中に微粒子が含まれている場合、微粒子の捕捉が行われる。 In the particle measuring method of the present embodiment, both the particle measuring device 12 and the filter 13 are operated (step S11). The particle measuring instrument 12 and the filter 13 do not necessarily have to be operated at the same time, as long as both the particle measuring instrument 12 and the filter 13 are in operation.
Here, the operating state of the particle measuring device means a state in which sample water is introduced into the particle measuring device and the particles contained in the sample water are measured by the particle measuring device. The operating state of the filter means a state in which pure water is introduced into the filter and sample water is filtered. At this time, when fine particles are contained in the sample water, the fine particles are captured.
　なお、濾過器１３の回転数、圧力、及び連続稼働時間（１サイクルの連続稼働時間、日数）は、対象となる試料水や、本開示に係る微粒子測定方法が適用される場所等に応じて、適宜選択される。 Note that the rotation speed, pressure, and continuous operation time (one cycle continuous operation time, days) of the filter 13 depend on the target sample water, the place where the particulate measurement method according to the present disclosure is applied, and the like. Are appropriately selected.
　次に、微粒子計測器１２による測定結果における異常の有無を確認する（ステップＳ１２）。この異常の有無は、上記制御部にて判定するようにしてもよい。
　例えば、微粒子計測器１２と制御部１４とが協働し、微粒子計測器１２による測定結果が制御部１４へ出力され、制御部１４が当該測定結果を異常か否か判定するように構成することができる。
　制御部１４による異常の有無の判定には、例えば、制御部１４と協働する記憶媒体に測定結果の正常値及び異常値を閾値や数値範囲を用いて記憶させておき、制御部１４が記憶媒体に記憶された、測定結果の正常値及び異常値のデータに基づき、判定することができる。
　また、微粒子計測器１２による測定結果の異常がすぐに解消する場合や、微粒子計測器１２自体の不具合による異常が確認される場合を考慮して、制御部１４は、微粒子が所定数以上かつ所定時間以上連続して測定された場合に異常と判定することが好ましい。これにより、微粒子計測器１２による微粒子の数及び大きさ等に起因する確実な異常のみを判定することができる。 Next, presence / absence of abnormality in the measurement result by the particle measuring instrument 12 is confirmed (step S12). The presence or absence of this abnormality may be determined by the control unit.
For example, the particle measuring instrument 12 and the control unit 14 cooperate to output a measurement result from the particle measuring instrument 12 to the control unit 14, and the control unit 14 determines whether or not the measurement result is abnormal. Can do.
For the determination of the presence / absence of abnormality by the control unit 14, for example, the normal value and the abnormal value of the measurement result are stored in a storage medium cooperating with the control unit 14 using a threshold value or a numerical range, and the control unit 14 stores the normal value. The determination can be made based on the normal value and abnormal value data of the measurement result stored in the medium.
Further, in consideration of the case where the abnormality of the measurement result by the particle measuring instrument 12 is resolved immediately or the case where the abnormality due to the defect of the particle measuring instrument 12 itself is confirmed, the control unit 14 has a predetermined number or more of the particles. It is preferable to determine that there is an abnormality when measured continuously for more than a time. Thereby, only the reliable abnormality resulting from the number and size of the fine particles by the fine particle measuring instrument 12 can be determined.
　ステップＳ１２で異常が確認された場合、濾過器１３により継続して濾過を行う（ステップＳ１３）。ステップＳ１２で異常が確認されなかった場合にも、微粒子計測器１２及び濾過器１３は稼働状態のままであり、これらを常時稼働しておく（ステップＳ１１）。
　なお、濾過器１３を「常時」稼働させておくことには、任意の時間（日数）を１サイクルとして連続で稼働させておくことが含まれる。濾過器１３の連続稼働の１サイクル終了後は、数十分（例えば３０分間）以内に濾過器１３の濾過膜を交換し、再度、連続稼働させることが好ましい。 When abnormality is confirmed by step S12, it filters by the filter 13 continuously (step S13). Even when no abnormality is confirmed in step S12, the fine particle measuring instrument 12 and the filter 13 remain in an operating state, and these are always operated (step S11).
It should be noted that keeping the filter 13 in operation at all times includes keeping the filter 13 in operation continuously at an arbitrary time (number of days). After completion of one cycle of continuous operation of the filter 13, it is preferable to replace the filter membrane of the filter 13 within several tens of minutes (for example, 30 minutes) and continuously operate again.
　微粒子計測器１２による測定結果に異常が確認された後に継続して稼働している濾過器１３を、所定後に停止する（ステップＳ１５）。
　濾過器１３を停止する時期としては、異常時の微粒子を濾過器１３により確実に捕捉するため、上記異常が解消したときとすることが好ましい（ステップＳ１４）。この場合、当該異常が解消したことを濾過器１３の停止条件とするために、当該異常が解消したか否かの判定が行われることが好ましい。この判定も上記制御部１４にて行うことが可能である。
　また、濾過器１３を停止する時期としては、異常が確認されてから、所定時間が経過した後又は所定濾過量を通水した後に設定することもできる。この所定時間又は所定濾過量としては、要求水質や対象となる試料水に応じて、異常が解消するのに十分な時間又は濾過量に設定することが好ましい。 The filter 13 that is continuously operating after an abnormality is confirmed in the measurement result by the particle measuring instrument 12 is stopped after a predetermined time (step S15).
The time for stopping the filter 13 is preferably set to the time when the abnormality is resolved in order to surely capture the abnormal particles by the filter 13 (step S14). In this case, it is preferable to determine whether or not the abnormality has been resolved so that the abnormality is resolved and the stop condition of the filter 13 is set. This determination can also be performed by the control unit 14.
In addition, the time when the filter 13 is stopped can be set after a predetermined time has passed after the abnormality is confirmed or after a predetermined amount of filtration has passed through. The predetermined time or the predetermined filtration amount is preferably set to a time or a filtration amount sufficient for eliminating the abnormality, depending on the required water quality and the target sample water.
　濾過器１３を停止した後は、濾過器１３から濾過膜を取り出し、濾過膜に捕捉された微粒子について、光学顕微鏡や走査型電子顕微鏡（ＳＥＭ）等を用いて、直接検鏡法による分析、測定を行う（ステップＳ１６）。
　直接検鏡法は、微粒子数を測定しようとする試料水（純水）を、測定したい大きさの微粒子を捕捉できる濾過膜で濾過し、微粒子を捕捉して顕微鏡で拡大して観察しながら計数し、試料に存在していた微粒子数を求める方法である。この直接検鏡法による測定は、ＪＩＳ　Ｋ０５５４（超純水中の微粒子測定方法）における「光学顕微鏡による測定方法」又は「走査型電子顕微鏡による測定方法」に準拠して行われる。
　また、走査型電子顕微鏡にエネルギー分散型Ｘ線分析装置（ＥＤＸ）等のＸ線分析装置が取り付けられた装置によって、微粒子を走査型電子顕微鏡で観察しながら、微粒子の組成を分析することもできる。 After stopping the filter 13, the filter membrane is taken out from the filter 13, and the microparticles captured by the filter membrane are analyzed and measured by a direct spectroscopic method using an optical microscope, a scanning electron microscope (SEM), or the like. Is performed (step S16).
In the direct spectroscopic method, sample water (pure water) for which the number of fine particles is to be measured is filtered through a filtration membrane that can capture the fine particles of the desired size, and the fine particles are captured and counted with a microscope for observation. In this method, the number of fine particles present in the sample is obtained. The measurement by the direct spectroscopic method is performed in accordance with “Measurement method using an optical microscope” or “Measurement method using a scanning electron microscope” in JIS K0554 (Method for measuring fine particles in ultrapure water).
In addition, the composition of the fine particles can be analyzed while observing the fine particles with a scanning electron microscope using an apparatus in which an X-ray analyzer such as an energy dispersive X-ray analyzer (EDX) is attached to the scanning electron microscope. .
　以上詳述したとおり、第１実施形態の微粒子測定方法及び微粒子測定システム１１によれば、微粒子計測器１２と、直接検鏡法による分析用の濾過器１３とを共に稼働させておき、微粒子計測器１２の測定結果に異常が認められた場合にも継続して濾過器１３を稼働させておくため、異常時に適時に微粒子を捕捉することができる。そのため、捕捉されない微粒子数を低減することができ、微粒子の捕捉量を多くすることが可能となる。そして、捕捉された微粒子は直接検鏡法にて詳細に分析され、微粒子計測器１２による測定結果の異常原因を迅速に調べることが可能となり、純水中の微粒子管理の質を向上することが可能となる。 As described in detail above, according to the particle measuring method and particle measuring system 11 of the first embodiment, the particle measuring instrument 12 and the filter 13 for analysis by the direct spectroscopic method are operated together to measure the particle. Even when an abnormality is recognized in the measurement result of the vessel 12, the filter 13 is continuously operated, so that the fine particles can be captured in a timely manner in the event of an abnormality. Therefore, the number of fine particles that are not captured can be reduced, and the amount of captured fine particles can be increased. The captured fine particles are analyzed in detail by a direct spectroscopic method, and it becomes possible to quickly investigate the cause of the abnormality in the measurement result by the fine particle measuring instrument 12, thereby improving the quality of fine particle management in pure water. It becomes possible.
　なお、本実施形態の微粒子測定システム１１において、微粒子計測器（計測部）１２及び濾過器（濾過部）１３に導入された純水は、排水されてもよいし、回収ラインを通り原水槽又は除濁水槽にて回収し、原水の一部として使用されてもよい。これは、第２実施形態及び第３実施形態の各実施形態における計測部及び濾過部に導入された純水についても同様である。 In the fine particle measurement system 11 of the present embodiment, the pure water introduced into the fine particle measuring instrument (measuring unit) 12 and the filter (filtering unit) 13 may be drained, passed through the recovery line, or the raw water tank or It collects in a turbidity water tank and may be used as a part of raw water. The same applies to the pure water introduced into the measuring unit and the filtering unit in each of the second and third embodiments.
＜第２実施形態＞
　第２実施形態に係る微粒子測定方法及び微粒子測定システムは、微粒子を直接検鏡法による分析用に捕捉する濾過部として、２つの濾過器が用いられる点で第１実施形態と異なる。 Second Embodiment
The fine particle measurement method and the fine particle measurement system according to the second embodiment are different from the first embodiment in that two filters are used as a filtration unit that captures fine particles for analysis by a direct spectroscopic method.
　第２実施形態に係る微粒子測定方法は、上記濾過部として、試料水（本実施形態では純水）の供給を互いに切り替え可能に設置された、第１濾過部（第１濾過器）と第２濾過部（第２濾過器）とが用いられる。
　そして、本実施形態の微粒子測定方法は、上記計測部として微粒子計測器と、第１濾過器とが共に稼働している状態で、微粒子計測器による測定結果に異常が認められた場合に、第１濾過器を停止すると共に、第２濾過器を稼働させるものである。
　本実施形態の微粒子測定方法では、第１濾過器と第２濾過器とを用いることで、純水の濾過を継続して行うようにしている。 In the fine particle measurement method according to the second embodiment, the first filtration unit (first filter) and the second filtration unit are installed so that the supply of sample water (pure water in this embodiment) can be switched to each other. A filtration unit (second filter) is used.
Then, the particle measuring method of the present embodiment is the first when the measurement result by the particle measuring instrument is found to be abnormal while the particle measuring instrument and the first filter are operating as the measuring unit. The first filter is stopped and the second filter is operated.
In the fine particle measurement method of the present embodiment, pure water is continuously filtered by using the first filter and the second filter.
　図３は、本実施形態の微粒子測定方法を適用した微粒子測定システム２１の一構成例（第２実施形態に係る微粒子測定システム２１）を示す系統図である。
　本実施形態の微粒子測定システム２１は、微粒子計測器１２、第１濾過器２３ａ、第２濾過器２３ｂ、及び制御部２４を備える。本実施形態では、微粒子計測器１２、第１濾過器２３ａ及び第２濾過器２３ｂは、貯槽１５に貯留された試料水（純水）Ｗが流れる配管１６から分岐して接続されている。 FIG. 3 is a system diagram showing a configuration example of the fine particle measurement system 21 to which the fine particle measurement method of the present embodiment is applied (the fine particle measurement system 21 according to the second embodiment).
The fine particle measurement system 21 of the present embodiment includes a fine particle measuring instrument 12, a first filter 23a, a second filter 23b, and a control unit 24. In the present embodiment, the particle measuring instrument 12, the first filter 23a, and the second filter 23b are branched and connected from the pipe 16 through which the sample water (pure water) W stored in the storage tank 15 flows.
　本実施形態で用いられる微粒子計測器１２は、第１実施形態で用いられる微粒子計測器１２と同様である。また、本実施形態で用いられる第１濾過器２３ａ及び第２濾過器２３ｂは、共に第１実施形態で用いられる濾過器１３と同様に説明されるものであるが、制御部２４による制御のされ方が第１実施形態とは異なる。なお、本実施形態においても第１濾過器２３ａ及び第２濾過器２３ｂとしては共に遠心濾過器２３ａ、２３ｂを用いているが、分離膜ユニット等の他の濾過器を用いることもできる。 The particle measuring instrument 12 used in the present embodiment is the same as the particle measuring instrument 12 used in the first embodiment. The first filter 23a and the second filter 23b used in the present embodiment are both described in the same manner as the filter 13 used in the first embodiment, but are controlled by the control unit 24. This is different from the first embodiment. In this embodiment, the centrifugal filters 23a and 23b are both used as the first filter 23a and the second filter 23b, but other filters such as a separation membrane unit may be used.
　本実施形態では、制御部２４は、少なくとも第１濾過器２３ａ及び第２濾過器２３ｂを制御する機能を有する。そして、制御部２４は、微粒子計測器１２と第１濾過器２３ａとが共に稼働している状態において、微粒子計測器１２による測定結果に異常が認められた場合に、第１濾過器２３ａを停止すると共に第２濾過器２３ｂを稼働させて、純水Ｗの濾過が継続して行われるように制御する部である。
　制御部２４は、第１濾過器２３ａ及び／又は第２濾過器２３ｂに備わっていてもよく、第１濾過器２３ａ及び第２濾過器２３ｂとは別途、設けられていてもよい。 In the present embodiment, the control unit 24 has a function of controlling at least the first filter 23a and the second filter 23b. And the control part 24 stops the 1st filter 23a, when abnormality is recognized in the measurement result by the particle measuring device 12, in the state which the particle measuring device 12 and the 1st filter 23a are working together. In addition, the second filter 23b is operated to control the pure water W to be continuously filtered.
The control unit 24 may be provided in the first filter 23a and / or the second filter 23b, and may be provided separately from the first filter 23a and the second filter 23b.
　また、制御部２４は、第１濾過器２３ａ及び第２濾過器２３ｂのほか、微粒子計測器１２を制御する機能を有していてもよい。
　例えば、微粒子計測器１２と制御部２４とが協働し、微粒子計測器１２による測定結果が制御部２４へ出力され、制御部２４が当該測定結果を異常か否か判定するように構成することができる。このように微粒子計測器１２と制御部２４とが協働することで、微粒子計測器１２による測定結果が異常か否かを正確かつ早く判断することができる。 In addition to the first filter 23a and the second filter 23b, the control unit 24 may have a function of controlling the particle measuring instrument 12.
For example, the particle measuring instrument 12 and the control unit 24 cooperate to output a measurement result from the particle measuring instrument 12 to the control unit 24, and the control unit 24 determines whether or not the measurement result is abnormal. Can do. As described above, the particle measuring instrument 12 and the control unit 24 cooperate to determine whether the measurement result by the particle measuring instrument 12 is abnormal or not accurately and quickly.
　制御部２４による異常の有無の判定には、例えば、制御部２４と協働する記憶媒体に測定結果の正常値及び異常値を記憶させておき、制御部２４が記憶媒体に記憶された、測定結果の正常値及び異常値のデータに基づき、判定することができる。
　また、微粒子計測器１２による測定結果の異常がすぐに解消する場合や、微粒子計測器１２自体の不具合による異常が確認される場合を考慮して、制御部２４は、微粒子が所定数以上かつ所定時間以上連続して測定された場合に異常と判定することが好ましい。これにより、微粒子計測器１２による微粒子の数及び大きさ等に起因する確実な異常のみを判定することができる。 In the determination of the presence or absence of abnormality by the control unit 24, for example, the normal value and the abnormal value of the measurement result are stored in a storage medium cooperating with the control unit 24, and the control unit 24 stores the measurement value in the storage medium. The determination can be made based on the normal value and abnormal value data of the result.
Further, in consideration of the case where the abnormality of the measurement result by the particle measuring instrument 12 is resolved immediately or the case where the abnormality due to the defect of the particle measuring instrument 12 itself is confirmed, the control unit 24 has a predetermined number of particles more than a predetermined number. It is preferable to determine that there is an abnormality when measured continuously for more than a time. Thereby, only the reliable abnormality resulting from the number and size of the fine particles by the fine particle measuring instrument 12 can be determined.
　制御部２４は、微粒子計測器１２による測定結果の異常が解消した場合に、継続して濾過を行うために稼働された第２濾過器２３ｂを停止し、停止中にあった第１濾過器２３ａを再び稼働させるように制御することができる。
　制御部２４がこのように第１濾過器２３ａ及び第２濾過器２３ｂを制御することで、微粒子計測器１２による測定結果が正常の場合には、第１濾過器２３ａで濾過を行うこととし、微粒子計測器１２による測定結果が異常の場合には、第２濾過器で濾過を行うことができる。そのため、第１濾過器２３ａは常時用、第２濾過器２３ｂは異常時用として使い分けることができる。 When the abnormality in the measurement result by the particle measuring instrument 12 is resolved, the control unit 24 stops the second filter 23b that has been operated in order to continuously perform filtration, and the first filter 23a that has been stopped. Can be controlled to operate again.
When the control unit 24 controls the first filter 23a and the second filter 23b in this way, and the measurement result by the fine particle measuring device 12 is normal, the first filter 23a performs filtration. When the measurement result by the fine particle measuring instrument 12 is abnormal, it can be filtered by the second filter. Therefore, the first filter 23a can be used for normal use and the second filter 23b can be used for abnormal use.
　第１濾過器２３ａを正常時用とし、第２濾過器２３ｂを異常時用とすることで、微粒子計測器１２による異常が解消した後は、第２濾過器２３ｂを停止し、その第２濾過器２３ｂの濾過膜を取り出して、濾過膜上に捕捉された微粒子の分析を行うことができる。そして、その間にも第１濾過器２３ａを稼働させておくことができ、正常時においても微粒子を捕捉することができる。 After the first filter 23a is used for normal conditions and the second filter 23b is used for abnormal conditions, the second filter 23b is stopped after the abnormality by the fine particle measuring instrument 12 has been resolved, and the second filtration is performed. The filtration membrane of the vessel 23b can be taken out and the fine particles captured on the filtration membrane can be analyzed. During this time, the first filter 23a can be operated, and fine particles can be captured even during normal operation.
　なお、制御部２４による第１濾過器２３ａ及び第２濾過器２３ｂの制御は、例えば、それぞれの濾過器２３ａ、２３ｂに対して、試料水Ｗの導入の切り替えによって行うことができる。より具体的には、各濾過器２３ａ、２３ｂにおいて試料水Ｗの導入側の配管１６に切り替え弁（不図示）を設けておき、制御部２４がその切り替え弁を制御することで、第１濾過器２３ａと第２濾過器２３ｂの停止及び稼働を行うようにすることができる。 In addition, control of the 1st filter 23a and the 2nd filter 23b by the control part 24 can be performed by switching introduction of the sample water W with respect to each filter 23a, 23b, for example. More specifically, in each filter 23a, 23b, a switching valve (not shown) is provided in the piping 16 on the introduction side of the sample water W, and the control unit 24 controls the switching valve so that the first filtration is performed. It is possible to stop and operate the filter 23a and the second filter 23b.
　図４は、本実施形態の微粒子測定方法を表すフローチャート図である。なお、このフローチャート図は、上述の本実施形態の微粒子測定システム２１の動作も表している。
　図４では、本実施形態の微粒子測定方法が開始される前提として、微粒子計測器１２及び第１濾過器２３ａに純水Ｗが導入されている状態をスタートとしている。 FIG. 4 is a flowchart showing the fine particle measurement method of the present embodiment. In addition, this flowchart figure also represents operation | movement of the fine particle measurement system 21 of this embodiment mentioned above.
In FIG. 4, as a premise that the fine particle measurement method of the present embodiment is started, a state in which pure water W is introduced into the fine particle measurement device 12 and the first filter 23 a is started.
　本実施形態の微粒子測定方法では、微粒子計測器１２及び第１濾過器２３ａの両方を稼働させておく（ステップＳ２１）。微粒子計測器１２と第１濾過器２３ａとは必ずしも同時に稼働させる必要はなく、微粒子計測器１２と第１濾過器２３ａとが共に稼働状態にあればよい。
　なお、第１濾過器（遠心濾過器）２３ａの回転数、濾過圧力、及び連続稼働の１サイクルは、対象となる試料水や、本開示に係る微粒子測定方法が適用される場所等に応じて、適宜設定することができる。 In the fine particle measurement method of this embodiment, both the fine particle measuring instrument 12 and the first filter 23a are operated (step S21). The particle measuring instrument 12 and the first filter 23a are not necessarily operated at the same time, and it is sufficient that both the particle measuring instrument 12 and the first filter 23a are in an operating state.
In addition, the rotation speed of the first filter (centrifugal filter) 23a, the filtration pressure, and one cycle of continuous operation depend on the target sample water, the place where the fine particle measurement method according to the present disclosure is applied, and the like. Can be set as appropriate.
　次に、微粒子計測器１２による測定結果において、異常の有無を確認する（ステップＳ２２）。この異常の有無は、第１実施形態で述べたのと同様に、制御部２４にて判定するようにしてもよく、制御部２４による判定に際しては、制御部２４と記憶媒体とが協働するように構成してもよい。
　また、第１実施形態と同様に、制御部２４は、微粒子が所定数以上かつ所定時間以上連続して測定された場合に異常と判定することが好ましい。これにより、微粒子計測器１２による微粒子の数及び大きさ等に起因する確実な異常のみを判定することができる。 Next, the presence / absence of abnormality is confirmed in the measurement result by the particle measuring instrument 12 (step S22). The presence or absence of this abnormality may be determined by the control unit 24 as described in the first embodiment, and the control unit 24 and the storage medium cooperate in the determination by the control unit 24. You may comprise as follows.
Similarly to the first embodiment, it is preferable that the control unit 24 determines that there is an abnormality when the fine particles are continuously measured for a predetermined number or more and for a predetermined time or more. Thereby, only the reliable abnormality resulting from the number and size of the fine particles by the fine particle measuring instrument 12 can be determined.
　ステップＳ２２で異常が認められた場合、第１濾過器２３ａを停止し、かつ第２濾過器２３ｂを稼働させる（ステップＳ２３）。これにより、微粒子計測器１２により異常が認められた場合にも、継続して濾過を行うようにしている。第１濾過器２３ａの停止、及び第２濾過器２３ｂの稼働は、制御部２４により第１濾過器２３ａ及び第２濾過器２３ｂを制御して行うことができる。なお、第２濾過器（第２遠心濾過器）２３ｂの回転数及び濾過圧力についても、適宜設定することができ、第１濾過器２３ａから引き続き濾過を行うという観点から、第１濾過器２３ａと同条件とすることが好ましい。 When abnormality is recognized by step S22, the 1st filter 23a is stopped and the 2nd filter 23b is operated (step S23). As a result, even when an abnormality is recognized by the particle measuring instrument 12, filtration is continuously performed. The stop of the first filter 23a and the operation of the second filter 23b can be performed by controlling the first filter 23a and the second filter 23b by the control unit 24. Note that the rotation speed and filtration pressure of the second filter (second centrifugal filter) 23b can also be set as appropriate. From the viewpoint of continuing filtration from the first filter 23a, the first filter 23a and It is preferable to use the same conditions.
　第１濾過器２３ａの停止と第２濾過器２３ｂの稼働とのタイミングは、第１濾過器２３ａを停止した直後に第２濾過器２３ｂを稼働させることが好ましく、第１濾過器２３ａの停止と第２濾過器２３ｂの稼働とを略同じタイミングで行うことがより好ましい。第１濾過器２３ａと第２濾過器２３ｂとがこのように連動することで、タイムロスを抑え、捕捉されない微粒子数（ロス数）を抑えると共に、微粒子の捕捉量を多くすることが可能となる。 As for the timing of the stop of the first filter 23a and the operation of the second filter 23b, the second filter 23b is preferably operated immediately after the first filter 23a is stopped, and the stop of the first filter 23a is More preferably, the operation of the second filter 23b is performed at substantially the same timing. Since the first filter 23a and the second filter 23b are interlocked in this way, it is possible to suppress time loss, reduce the number of particles not captured (loss number), and increase the amount of captured particles.
　なお、ステップＳ２２で異常が確認されなかった場合にも、微粒子計測器１２及び第１濾過器２３ａは稼働状態のままであり、これらは正常時において常時稼働状態としておく（ステップＳ２１）。 Even if no abnormality is confirmed in step S22, the fine particle measuring instrument 12 and the first filter 23a remain in an operating state, and these are always in an operating state during normal operation (step S21).
　次に、微粒子計測器１２による測定結果に異常が確認された後に継続して稼働している第２濾過器２３ｂを、所定後に停止すると共に、第１濾過器２３ａを再び稼働させる（ステップＳ２５）。
　第２濾過器２３ｂを停止するタイミングとしては、異常時の微粒子を第２濾過器２３ｂにより確実に捕捉するため、上記異常が解消したときとすることが好ましい。この場合、当該異常が解消したことを第２濾過器２３ｂの停止条件とするために、当該異常が解消したか否かの判定を行うことが好ましい（ステップＳ２４）。この判定も上記制御部２４にて行うことが可能である。
　また、第２濾過器２３ｂを停止するタイミングとしては、異常確認後、所定時間が経過された後に設定することもできる。この所定時間としては、要求水質や対象となる試料水に応じて、異常が解消するのに十分な時間に設定することが好ましい。 Next, after the abnormality is confirmed in the measurement result by the particle measuring instrument 12, the second filter 23b continuously operating is stopped after a predetermined time, and the first filter 23a is operated again (step S25). .
The timing of stopping the second filter 23b is preferably when the abnormality is resolved in order to reliably capture the abnormal particles by the second filter 23b. In this case, it is preferable to determine whether or not the abnormality has been resolved in order to use the second filter 23b as a stop condition that the abnormality has been eliminated (step S24). This determination can also be performed by the control unit 24.
In addition, the timing for stopping the second filter 23b can be set after a predetermined time has elapsed after confirmation of the abnormality. The predetermined time is preferably set to a time sufficient for eliminating the abnormality, depending on the required water quality and the target sample water.
　第２濾過器２３ｂを停止した後は、第２濾過器２３ｂから濾過膜を取り出し、濾過膜上に捕捉された微粒子について、第１実施形態で述べた方法と同様に、直接検鏡法にて、微粒子の数、大きさ（粒径）、及び組成等の分析及び測定を行う（ステップＳ２６）。 After stopping the second filter 23b, the filtration membrane is taken out from the second filter 23b, and the microparticles captured on the filtration membrane are directly examined by the microscopic method as in the method described in the first embodiment. Then, analysis and measurement of the number, size (particle size), composition, and the like of the fine particles are performed (step S26).
　以上詳述したとおり、第２実施形態の微粒子測定方法及び微粒子測定システム２１によれば、微粒子計測器１２と第１濾過器２３ａとを共に稼働させておき、微粒子計測器１２の測定結果に異常が認められた場合に、第１濾過器２３ａを停止し、かつ第２濾過器２３ｂを稼働させるため、異常時に適時に微粒子を捕捉することができる。そのため、捕捉されない微粒子数を低減することができ、微粒子の捕捉量を多くすることが可能となる。そして、捕捉された微粒子は直接検鏡法にて詳細に分析され、微粒子計測器１２による測定結果の異常原因を迅速に調べることが可能となり、純水中の微粒子管理の質を向上することが可能となる。
　また、第１濾過器２３ａを常時用、第２濾過器２３ｂを異常時用とすることで、第２濾過器２３ｂにより捕捉された微粒子を直接検鏡法にて分析している間にも、第１濾過器２３ａを稼働させておくことができ、純水中の微粒子を常時モニタリングすることが可能となる。 As described above in detail, according to the fine particle measurement method and the fine particle measurement system 21 of the second embodiment, both the fine particle measuring device 12 and the first filter 23a are operated, and the measurement result of the fine particle measuring device 12 is abnormal. Is recognized, the first filter 23a is stopped and the second filter 23b is operated, so that it is possible to capture fine particles in a timely manner in an abnormal state. Therefore, the number of fine particles that are not captured can be reduced, and the amount of captured fine particles can be increased. The captured fine particles are analyzed in detail by a direct spectroscopic method, and it becomes possible to quickly investigate the cause of the abnormality in the measurement result by the fine particle measuring instrument 12, thereby improving the quality of fine particle management in pure water. It becomes possible.
In addition, while the first filter 23a is always used and the second filter 23b is used for an abnormal time, while the microparticles captured by the second filter 23b are directly analyzed by the microscopic method, The first filter 23a can be operated, and it is possible to constantly monitor fine particles in pure water.
＜第３実施形態＞
　次に、本開示の微粒子測定方法及び微粒子測定システムを超純水製造システムに用いる実施形態を例示して説明する。 <Third Embodiment>
Next, an embodiment in which the fine particle measurement method and the fine particle measurement system of the present disclosure are used in an ultrapure water production system will be described as an example.
　図５は、本実施形態に係る超純水製造設備１００を説明するための一構成例を示す系統図である。本実施形態で説明する超純水製造設備１００は、一次純水製造システム１０１、及び超純水製造システム（サブシステム及び二次純水製造システムとも称される。）１０２を備える。
　この超純水製造設備１００は、一次純水製造システム１０１にて製造された純水をさらに超純水製造システム１０２にて精製処理し、超純水を製造する設備である。 FIG. 5 is a system diagram showing a configuration example for explaining the ultrapure water production facility 100 according to the present embodiment. An ultrapure water production facility 100 described in the present embodiment includes a primary pure water production system 101 and an ultrapure water production system (also referred to as a subsystem and a secondary pure water production system) 102.
This ultrapure water production facility 100 is a facility for producing ultrapure water by further purifying the pure water produced by the primary pure water production system 101 using the ultrapure water production system 102.
　一次純水製造システム（一次純水製造工程）１０１は、超純水製造システム（超純水製造工程）１０２の前段階に位置し、超純水製造システム１０２に試料水（純水）Ｗを導入するための装置である。一次純水製造システム１０１の前段階には、通常、前処理装置（前処理工程／不図示）を有している。前処理工程では、被処理水となる原水（工業用水、市水及び井水等）中に含まれる懸濁物質の大部分と有機物の一部を除去し、後段の一次純水製造工程の負荷を低減することが行われる。前処理装置の構成は、特に限定されるものではなく、凝集濾過、凝集沈殿濾過、凝集加圧浮上濾過、及び膜式濾過等が用いられる。
　一次純水製造システム１０１の構成も、特に限定されるものではなく、逆浸透（ＲＯ）膜分離装置、イオン交換装置、脱塩装置、吸着装置、有機物分解装置（紫外線酸化装置等）、脱気装置、及び殺菌装置等を任意の順で配置することができる。 The primary pure water production system (primary pure water production process) 101 is located in the previous stage of the ultra pure water production system (ultra pure water production process) 102, and sample water (pure water) W is supplied to the ultra pure water production system 102. It is a device for introduction. The pre-stage of the primary pure water production system 101 usually has a pre-treatment device (pre-treatment process / not shown). In the pretreatment process, most of the suspended solids and part of the organic matter contained in the raw water (industrial water, city water, well water, etc.) to be treated are removed, and the load of the primary pure water production process in the subsequent stage Is performed. The configuration of the pretreatment device is not particularly limited, and flocculation filtration, flocculation precipitation filtration, flocculation pressure flotation filtration, membrane filtration, and the like are used.
The configuration of the primary pure water production system 101 is also not particularly limited, and is a reverse osmosis (RO) membrane separation device, an ion exchange device, a desalination device, an adsorption device, an organic matter decomposition device (such as an ultraviolet oxidation device), and a deaeration Devices, sterilizers, etc. can be arranged in any order.
　超純水製造システム（超純水製造工程）１０２は、一次純水製造工程１０１で得られた純水Ｗをさらに高純度に精製処理するものであり、一般的に、熱交換器、紫外線酸化装置、イオン交換装置、及び限外濾過装置等を組み合わせて構成される。
　本実施形態の超純水製造システム１０２は、一次純水製造システム１０１で製造された一次純水Ｗを配管１０３ａから貯槽１０４に受け、給水ポンプ１０５で引き、熱交換器１０６、低圧紫外線酸化装置１０７、脱気装置１０８、イオン交換装置１０９、及び限外濾過（ＵＦ）膜装置１１０で順次処理するものである。そして、この超純水製造システム１０２は、各処理で得られた超純水を配管１０３ｂによりユースポイント１１１に送り、余剰水を配管１０３ｃにより貯槽１０４に戻すものである。 The ultrapure water production system (ultrapure water production process) 102 purifies the pure water W obtained in the primary pure water production process 101 to a higher purity, and generally includes a heat exchanger, ultraviolet oxidation. A device, an ion exchange device, an ultrafiltration device, and the like are combined.
The ultrapure water production system 102 of this embodiment receives the primary pure water W produced by the primary pure water production system 101 from the pipe 103a to the storage tank 104, draws it with the water supply pump 105, heat exchanger 106, low-pressure ultraviolet oxidizer. 107, deaeration device 108, ion exchange device 109, and ultrafiltration (UF) membrane device 110 are sequentially processed. And this ultrapure water manufacturing system 102 sends the ultrapure water obtained by each process to the use point 111 by the piping 103b, and returns surplus water to the storage tank 104 by the piping 103c.
　超純水製造システム１０２には、本開示の微粒子測定システム３１が設けられている。超純水製造システム１０２における微粒子測定システム３１の設置場所は、特に限定されない。本実施形態では、超純水製造システム１０２におけるＵＦ膜装置１１０の後段に、ＵＦ膜装置１１０の処理水（超純水）が通る配管１０３ｂを分岐して、微粒子測定システム２１が設けられている。そして、ＵＦ膜装置１１０の処理水（超純水）が微粒子測定システム３１に導入されるように構成されている。 The ultrapure water production system 102 is provided with the particulate measurement system 31 of the present disclosure. The installation location of the particulate measurement system 31 in the ultrapure water production system 102 is not particularly limited. In the present embodiment, a particulate measurement system 21 is provided by branching a pipe 103b through which treated water (ultra pure water) of the UF membrane device 110 passes after the UF membrane device 110 in the ultra pure water production system 102. . Then, the treated water (ultra pure water) of the UF membrane device 110 is configured to be introduced into the fine particle measurement system 31.
　微粒子測定システム３１は、微粒子計測器（計測部）３２と、濾過器（濾過部）３３ａ、３３ｂと、制御部（不図示）とを有する。濾過器３３ａ、３３ｂとしては、上記第２実施形態の微粒子測定方法及び微粒子測定システムに適用可能な第１遠心濾過器３３ａ及び第２遠心濾過器３３ｂを用いることができる。第１濾過器３３ａ及び第２濾過器３３ｂの動作は、上記第２実施形態で述べたのと同様である。
　なお、第１実施形態で述べた微粒子測定方法及び微粒子測定システムを図５に示すような超純水製造設備１００（超純水製造システム１０２）に適用する場合は、第２濾過器３３ｂを外せばよい。 The fine particle measurement system 31 includes a fine particle measuring instrument (measuring unit) 32, filters (filtering units) 33a and 33b, and a control unit (not shown). As the filters 33a and 33b, the first centrifugal filter 33a and the second centrifugal filter 33b applicable to the fine particle measurement method and the fine particle measurement system of the second embodiment can be used. The operations of the first filter 33a and the second filter 33b are the same as those described in the second embodiment.
When applying the fine particle measurement method and the fine particle measurement system described in the first embodiment to the ultrapure water production facility 100 (ultra pure water production system 102) as shown in FIG. 5, the second filter 33b should be removed. That's fine.
　また、図５に示す超純水製造設備１００（超純水製造システム１０２）では、第１遠心濾過器３３ａ及び第２遠心濾過器３３ｂの代わりに、通気圧（給水圧）を用いた分離膜ユニット（第１分離膜ユニット３３ｃ及び第２分離膜ユニット３３ｄ）を用いることもできる（図５において括弧で示す。）。分離膜ユニット３３ｃ、３３ｄを用いる場合、分離膜ユニット３３ｃ、３３ｄによる濾過の停止及び稼働を切り替え可能な開閉弁３３１、３３２を設けるのが好適である。
　この場合、第１分離膜ユニット３３ｃを常時稼働用とし、第２分離膜ユニット３３ｄを異常時稼働用とする。そして、微粒子計測器３２及び第１分離膜ユニット３３ｃの稼働状態において、微粒子計測器３２による測定結果で異常が認められた場合、第１分離膜ユニット３３ｃの後段の第１開閉弁３３１を開から閉にすると共に、停止状態にあった第２分離膜ユニット３３ｄの後段の第２開閉弁３３２を閉から開にする。第１開閉弁３３１及び第２開閉弁３３２は、共に制御部（不図示）にて制御することができ、制御部は、微粒子計測器３２と協働することで、第１開閉弁３３１及び第２開閉弁３３２を自動で開閉することができる。 Further, in the ultrapure water production facility 100 (ultrapure water production system 102) shown in FIG. 5, a separation membrane using aeration pressure (feed water pressure) instead of the first centrifugal filter 33a and the second centrifugal filter 33b. Units (first separation membrane unit 33c and second separation membrane unit 33d) can also be used (shown in parentheses in FIG. 5). When the separation membrane units 33c and 33d are used, it is preferable to provide on-off valves 331 and 332 that can switch between the stop and operation of filtration by the separation membrane units 33c and 33d.
In this case, the first separation membrane unit 33c is always used for operation, and the second separation membrane unit 33d is used for abnormal operation. In the operating state of the particle measuring instrument 32 and the first separation membrane unit 33c, if an abnormality is recognized in the measurement result by the particle measuring instrument 32, the first on-off valve 331 at the rear stage of the first separation membrane unit 33c is opened. In addition to closing, the second on-off valve 332 at the rear stage of the second separation membrane unit 33d in the stopped state is opened from the closed state. Both the first on-off valve 331 and the second on-off valve 332 can be controlled by a control unit (not shown), and the control unit cooperates with the fine particle measuring device 32 to provide the first on-off valve 331 and the second on-off valve 332. The two on-off valve 332 can be opened and closed automatically.
　以上詳述したとおり、第３実施形態の超純水製造システム１０２（超純水製造設備１００）によれば、本開示に係る微粒子測定システム３１を備えるため、その微粒子測定システム３１が有する効果を奏することができる。加えて、その微粒子測定システム３１により、適時に微粒子を捕捉可能であることから、製造される超純水の水質（品質）をより高めることが可能となる。よって、本実施形態の超純水製造システム１０２は、半導体製造分野及び医薬品製造分野等の様々な工業分野において、好適に用いられる。 As described above in detail, according to the ultrapure water production system 102 (ultrapure water production facility 100) of the third embodiment, since the fine particle measurement system 31 according to the present disclosure is provided, the effects of the fine particle measurement system 31 are provided. Can play. In addition, since the fine particle measurement system 31 can capture the fine particles in a timely manner, it is possible to further improve the quality (quality) of the manufactured ultrapure water. Therefore, the ultrapure water production system 102 of the present embodiment is suitably used in various industrial fields such as the semiconductor manufacturing field and the pharmaceutical manufacturing field.
　なお、本開示の微粒子測定方法及び微粒子測定システムは、次のように構成することも可能である。
　上記実施形態で例示した微粒子測定システムには、水質をモニタリングする部として、溶存ガス濃度計、ＴＯＣ計、過酸化水素濃度計、シリカ計、ホウ素計、蒸発残査計、及び水温計等の種々の計測器を設けることも可能である。
　第２実施形態及び第３実施形態では、濾過器を２つ備える構成を例示したが、濾過器の数は２以上としてもよい。この場合、各濾過器を制御可能な制御部を備えるのが好ましい。 Note that the fine particle measurement method and the fine particle measurement system of the present disclosure can be configured as follows.
In the fine particle measurement system exemplified in the above embodiment, various parts such as a dissolved gas concentration meter, a TOC meter, a hydrogen peroxide concentration meter, a silica meter, a boron meter, an evaporation residue meter, and a water temperature meter are used as a unit for monitoring water quality. It is also possible to provide a measuring instrument.
In 2nd Embodiment and 3rd Embodiment, although the structure provided with two filters was illustrated, the number of filters is good also as 2 or more. In this case, it is preferable to provide a control unit capable of controlling each filter.
　本発明は、以下の構成を採用することも可能である。
［１］　試料水中の微粒子を測定する計測部と、前記試料水を濾過し、前記微粒子を直接検鏡法による分析用に捕捉する濾過部と、を共に稼働させておき、前記計測部の測定結果に異常が認められた場合にも、継続して前記試料水を濾過する工程を行う、微粒子測定方法。
［２］　前記計測部の測定結果に異常が認められた場合にも、前記濾過部を継続して稼働させる、上記［１］記載の微粒子測定方法。
［３］　前記濾過部は、前記試料水の供給を切り替え可能に設置された第１濾過部と第２濾過部とを有し、前記計測部と前記第１濾過部とが共に稼働している状態で、前記計測部による測定結果に異常が認められた場合に、前記第１濾過部を停止すると共に、前記第２濾過部を稼働させる、上記［１］記載の微粒子測定方法。
［４］　前記計測部による測定結果に異常が認められた後に継続して濾過が行われている濾過部を、前記異常が解消した後に停止する、上記［１］～［３］の何れか１つに記載の微粒子測定方法。
［５］　前記計測部による測定結果に異常が認められた後に継続して濾過が行われている濾過部により捕捉された微粒子の分析を行う、上記［１］～［４］の何れか１つに記載の微粒子測定方法。
［６］　前記計測部によって、前記微粒子が所定数以上かつ所定時間連続して測定された場合に前記異常と判定する、上記［１］～［５］の何れか１つに記載の微粒子測定方法。
［７］　上記［１］～［６］の何れか１つに記載の微粒子測定方法を用いる微粒子測定システム。
［８］　試料水中の微粒子を測定する計測部と、前記試料水を濾過し、前記微粒子を直接検鏡法による分析用に捕捉する濾過部と、前記計測部と前記濾過部とが共に稼働している状態で、前記計測部による測定結果に異常が認められた場合に、前記試料水の濾過が継続して行われるように制御する制御部と、を備える、微粒子測定システム。
［９］　前記制御部は、前記計測部による測定結果に異常が認められた場合にも、前記濾過部を継続して稼働させる、上記［８］記載の微粒子測定システム。
［１０］　前記濾過部は、前記純水の供給を切り替え可能に設置された第１濾過部と第２濾過部とを有し、前記制御部は、前記計測部と前記第１濾過部とが共に稼働している状態で、前記計測部による測定結果に異常が認められた場合に、前記第１濾過部を停止すると共に前記第２濾過部を稼働させる、上記［８］記載の微粒子測定システム。
［１１］　前記制御部は、前記計測部による測定結果に異常が認められた後に継続して濾過が行われている濾過部を、前記異常が解消した後に停止する、上記［８］～［１０］の何れか１つに記載の微粒子測定システム。
［１２］　前記制御部は、前記計測部によって、前記微粒子が所定数以上かつ所定時間連続して測定された場合に前記異常と判定する、上記［８］～［１１］の何れか１つに記載の微粒子測定システム。
［１３］　上記［１］～［６］の何れか１つに記載の微粒子測定方法を超純水製造工程において用いる超純水製造システム。
［１４］　上記［８］～［１２］の何れか１つに記載の微粒子測定システムを超純水の製造工程において備える超純水製造システム。 The present invention can also employ the following configurations.
[1] The measurement unit that measures the fine particles in the sample water and the filtration unit that filters the sample water and captures the fine particles for direct spectroscopic analysis are operated together to measure the measurement unit. A method for measuring fine particles, wherein the step of continuously filtering the sample water is performed even when abnormality is found in the result.
[2] The fine particle measurement method according to [1], wherein the filtration unit is continuously operated even when an abnormality is recognized in the measurement result of the measurement unit.
[3] The filtration unit includes a first filtration unit and a second filtration unit that are installed so that the supply of the sample water can be switched, and the measurement unit and the first filtration unit are both operating. In the state, when an abnormality is recognized in the measurement result by the measurement unit, the first filtration unit is stopped and the second filtration unit is operated.
[4] Any one of the above-mentioned [1] to [3], wherein the filtration unit that is continuously filtered after an abnormality is recognized in the measurement result by the measurement unit is stopped after the abnormality is resolved. The method for measuring fine particles according to 1.
[5] Any one of the above-mentioned [1] to [4], wherein fine particles captured by the filtration unit that is continuously filtered after an abnormality is recognized in the measurement result by the measurement unit are analyzed. 2. The method for measuring fine particles according to 1.
[6] The fine particle measurement method according to any one of [1] to [5], wherein the abnormality is determined when the measurement unit continuously measures the fine particles for a predetermined number or more and for a predetermined time. .
[7] A fine particle measurement system using the fine particle measurement method according to any one of [1] to [6].
[8] A measurement unit that measures fine particles in sample water, a filtration unit that filters the sample water and captures the fine particles for direct spectroscopic analysis, and the measurement unit and the filtration unit operate together. And a control unit that controls the sample water to be continuously filtered when an abnormality is recognized in the measurement result by the measurement unit.
[9] The fine particle measurement system according to [8], wherein the control unit continuously operates the filtration unit even when an abnormality is found in the measurement result by the measurement unit.
[10] The filtration unit includes a first filtration unit and a second filtration unit that are installed so that the supply of the pure water can be switched, and the control unit includes the measurement unit and the first filtration unit. The particulate measurement system according to [8] above, wherein when the abnormality is recognized in the measurement result by the measurement unit in a state where both are operating, the first filtration unit is stopped and the second filtration unit is operated. .
[11] The control unit stops the filtering unit that is continuously filtered after an abnormality is recognized in the measurement result by the measuring unit, after the abnormality is resolved, ] The fine particle measuring system according to any one of the above.
[12] In any one of the above [8] to [11], the control unit may determine that the abnormality is detected when the measurement unit continuously measures the fine particles for a predetermined number or more and for a predetermined time. The particulate measurement system described.
[13] An ultrapure water production system using the fine particle measurement method according to any one of [1] to [6] in an ultrapure water production process.
[14] An ultrapure water production system comprising the fine particle measurement system according to any one of [8] to [12] in an ultrapure water production process.
１１、２１、３１　微粒子測定システム
１２　微粒子計測器
１３　濾過器
２３ａ　第１濾過器
２３ｂ　第２濾過器
１４、２４　制御部
１００　超純水製造設備
１０１　一次純水製造システム
１０２　超純水製造システム 11, 21, 31 Fine particle measuring system 12 Fine particle measuring device 13 Filter 23a First filter 23b Second filter 14, 24 Control unit 100 Ultrapure water production facility 101 Primary pure water production system 102 Ultrapure water production system

Claims (11)

  1. 　試料水中の微粒子を測定する計測部と、前記試料水を濾過し、前記微粒子を直接検鏡法による分析用に捕捉する濾過部と、を共に稼働させておき、
    　前記計測部の測定結果に異常が認められた場合にも、継続して前記試料水を濾過する工程を行う、微粒子測定方法。     A measurement unit that measures fine particles in the sample water and a filtration unit that filters the sample water and captures the fine particles for direct spectroscopic analysis are operated together,
    A method for measuring fine particles, wherein the step of continuously filtering the sample water is performed even when an abnormality is recognized in the measurement result of the measurement unit.
  2. 　前記計測部の測定結果に異常が認められた場合にも、前記濾過部を継続して稼働させる、請求項１記載の微粒子測定方法。 The fine particle measurement method according to claim 1, wherein the filtration unit is continuously operated even when an abnormality is recognized in the measurement result of the measurement unit.
  3. 　前記濾過部は、前記試料水の供給を切り替え可能に設置された第１濾過部と第２濾過部とを有し、
    　前記計測部と前記第１濾過部とが共に稼働している状態で、前記計測部による測定結果に異常が認められた場合に、前記第１濾過部を停止すると共に、前記第２濾過部を稼働させる、請求項１記載の微粒子測定方法。     The filtration unit has a first filtration unit and a second filtration unit installed so as to be able to switch the supply of the sample water,
    When the measurement unit and the first filtration unit are operating together and an abnormality is recognized in the measurement result by the measurement unit, the first filtration unit is stopped and the second filtration unit is The fine particle measurement method according to claim 1, wherein the fine particle measurement method is operated.
  4. 　前記計測部による測定結果に異常が認められた後に継続して濾過が行われている濾過部を、前記異常が解消した後に停止する、請求項１～３の何れか１項記載の微粒子測定方法。 The fine particle measurement method according to any one of claims 1 to 3, wherein a filtration unit that is continuously filtered after an abnormality is recognized in a measurement result by the measurement unit is stopped after the abnormality is resolved. .
  5. 　前記計測部による測定結果に異常が認められた後に継続して濾過が行われている濾過部により捕捉された微粒子の分析を行う、請求項１～４の何れか１項記載の微粒子測定方法。 The fine particle measurement method according to any one of claims 1 to 4, wherein the fine particles captured by the filtration unit that is continuously filtered after an abnormality is recognized in the measurement result by the measurement unit are analyzed.
  6. 　試料水中の微粒子を測定する計測部と、
    　前記試料水を濾過し、前記微粒子を直接検鏡法による分析用に捕捉する濾過部と、
    　前記計測部と前記濾過部とが共に稼働している状態で、前記計測部による測定結果に異常が認められた場合に、前記試料水の濾過が継続して行われるように制御する制御部と、
    　を備える、微粒子測定システム。     A measurement unit for measuring fine particles in the sample water;
    A filtration unit for filtering the sample water and capturing the fine particles for analysis by direct microscopic method;
    A control unit that controls the sample water to be continuously filtered when an abnormality is found in the measurement result of the measurement unit while the measurement unit and the filtration unit are operating together. ,
    A fine particle measurement system comprising:
  7. 　前記制御部は、前記計測部による測定結果に異常が認められた場合にも、前記濾過部を継続して稼働させる、請求項６記載の微粒子測定システム。 The fine particle measurement system according to claim 6, wherein the control unit continuously operates the filtration unit even when an abnormality is recognized in the measurement result by the measurement unit.
  8. 　前記濾過部は、前記試料水の供給を切り替え可能に設置された第１濾過部と第２濾過部とを有し、
    　前記制御部は、前記計測部と前記第１濾過部とが共に稼働している状態で、前記計測部による測定結果に異常が認められた場合に、前記第１濾過部を停止すると共に前記第２濾過部を稼働させる、請求項６記載の微粒子測定システム。     The filtration unit has a first filtration unit and a second filtration unit installed so as to be able to switch the supply of the sample water,
    The control unit stops the first filtering unit and stops the first filtering unit when an abnormality is recognized in the measurement result by the measuring unit in a state where the measuring unit and the first filtering unit are operating together. The fine particle measurement system according to claim 6, wherein two filtration units are operated.
  9. 　前記制御部は、前記計測部による測定結果に異常が認められた後に継続して濾過が行われている濾過部を、前記異常が解消した後に停止する、請求項６～８の何れか１項記載の微粒子測定システム。 The control unit according to any one of claims 6 to 8, wherein the control unit stops the filtration unit that is continuously filtered after an abnormality is recognized in the measurement result by the measurement unit after the abnormality is resolved. The particulate measurement system described.
  10. 　前記制御部は、前記計測部によって、前記微粒子が所定数以上かつ所定時間連続して測定された場合に前記異常と判定する、請求項６～９の何れか１項記載の微粒子測定システム。 The fine particle measurement system according to any one of claims 6 to 9, wherein the control unit determines that the abnormality is present when the measurement unit continuously measures the fine particles for a predetermined number of times and for a predetermined time.
  11. 　請求項６～１０の何れか１項記載の微粒子測定システムを超純水の製造工程に備える超純水製造システム。 An ultrapure water production system comprising the fine particle measurement system according to any one of claims 6 to 10 in a production process of ultrapure water.
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